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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 C. E. Armantrout, H. Kato, M. I. Copeland

The data collected during this investigation indicate that the chromiumgadolinium system has extensive liquid immiscibility and one eutectic point . Liquid immiscibility occurred at temperatures above the monotectic isotherm , 1,830 ° C , which extended from less than 0.25 to about 85 weight - percent gadolinium . The eutectic was at 96 percent gadolinium and 1,170 ° C. Gadolinium and chromium were the only phases in this system . There was a solid solubility of less than 0.25 percent gadolinium in chromium at 1,730 ° C and less than 0.10 percent chromium in gadolinium at 1,160 ° C. The alloys were prepared by nonconsumable - electrode arc - melting , and the alloy system was investigated by heat treatment , metallography , thermal analysis , and X- ray diffraction . All the melting , heat treatments , and thermal analyses were conducted in a vacuum or in helium because of the reactivity of chromium and gadolinium with the components present in the atmosphere at elevated temperatures .

Jan 1, 1964

By Donald O. Rausch, Robert H. Merrill, David W. Wisecarver, S. Jackson Hubbard

Results are reported for stress - relief borehole - deformation measurements made in three underground openings near open - pit mines in the Ruth mining district , Nevada . A total of 134 deformation measurements were made in 8 boreholes . These measurements determined the regional stresses in the horizons above , below, and at the elevation of nearby open - pit mine floors ; knowledge of these stress conditions is considered essential information relative to certain aspects in the designing of stable pit slopes . The determinations indicate that the stresses in the district are due to the gravitational load of the overburden in a confined stress field .

Jan 1, 1964

By W. C. Wahl, M. M. Fine

Leonardite , a naturally occurring , partially oxidized form of lignite with a high content of humic acids , was investigated as a binder for iron ore pellets . Although insoluble in original condition , leonardite forms watersoluble salts with good binding properties when treated with certain alkalis such as sodium hydroxide . Soluble leonardite imparts excellent dry strength to pellets , but green strength is somewhat lower than that obtainable with bentonite . However , green strength can be improved by adding a small amount of calcium hydroxide to the leonardite - concentrate mixture . Leonardite binders were used successfully on three of the four different concentrates tested .

Jan 1, 1964

By R. W. Van Dolah, N. E. Hanna, F. C. Gibson

Measures that were taken to eliminate noise resulting from explosives work at the Bureau of Mines facility at Bruceton , Pa . , are described . A method for monitoring sound transmission characteristics of the atmosphere and control of the explosives testing is presented as a noise control measure that offered partial relief during the period in which the modifications were made . Design details of the replacement gallery , used for permissibility testing of explosives , and the modifications of four types of bombproofs are given . Operation of the closed facilities are completely satisfactory , and the noise problem has been entirely eliminated .

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 R. T. Johansen, R. J. Heemstra

In water flooding the gradual accumulation of insoluble materials on the sand face causes the injection pressures to increase while decreasing the amount of water injected . This plugging material often is composed primarily of insoluble precipitates of calcium , iron , and magnesium . Treatment with sodium tripolyphosphate ( STP ) either eliminates or reduces the formation of precipitates . Field tests are discussed showing the almost immediate effects of using STP in the injection water . Methods of treatment , solubility of STP in fresh water and brines , and precautions to observe when starting to treat a waterflood with this chemical are given . Laboratory data show that the preferential wettability of a crude oil for reservoir rock can be reversed by adding a small amount of STP to the flooding water . This reversal in wetting tendency should not only decrease the injection pressures but also increase oil recovery by improving the sweep efficiency of a water flood .

Jan 1, 1964

By George R. McCormick

Because several new and unusual synthetic minerals were found in the system MgO-MgF₂ - SiO2 with Li * , or Nat a similar system with Geo₂ replacing Sio , plus Lit was investigated . In addition to the expected compounds of germanium , Ge - fluor - hectorite and a Ge - fluor- chrysotile were synthesized . Protoamphibole was not observed . Data are given for 69 compositions prepared in the system MgO- MgF₂ - Ge02 at 6.94 percent LiF .

Jan 1, 1964

By K. K. Kelley, W. W. Weller

Heat capacity measurements of lead molybdate and lead tungstate were conducted over the temperature range from 51 ° to 298 ° K. The entropies were found to be S298.15 = 39.7 ± 0.5 cal / deg mole for lead molybdate and S298.15 = 40.2 ± 0.5 cal / deg mole for lead tungstate . The entropy values were combined with other pertinent data to obtain the entropies of formation of the two compounds from their constituent elements and oxides .

Jan 1, 1964

By Roy L. Wilfong, LeRoy R. Furlong, Louis P. Domingues

The bulk and apparent densities , particle size , and surface area of ceria powders derived from the ammonium sulfate , carbonate , nitrate , oxalate , and sulfate salts and heated at 950 ° to 1,500 ° C for 1 to 24 hours were studied . The bulk and apparent densities and particle size generally increased , and surface area decreased with increase in temperature and time of heating ; surface area was more sensitive to changes in temperature and time than the other properties studied . These properties of the ceria powders had a marked dependence on temperature and a lesser dependence on duration of heating at a given temperature ; and the source of oxide and thermal treatment cannot be considered optional in the preparation of refractory powders by thermal decomposition . The ammonium sulfate and sulfate salts heated at 950 ° and 1,200 ° C produced oxide powders with the lowest bulk density , the smallest particle size , and the highest surface area . The highest apparent densities were achieved for oxides resulting from the carbonate and the sulfate but the carbonate - derived material was considerably coarser . The surface areas of ceria powders derived from cerium salts decrease in the order of sulfate , ammonium sulfate , nitrate , oxalate , and carbonate . The observation of these physical properties are useful in predicting the sintering behavior of various oxide powders .

Jan 1, 1964

By Scott W. Hazen, George W. Gladfelter

This report presents the results of an initial investigation into some problems resulting from the use of assays representing unequal sample interval lengths and the use of the weighted average grade of ore in evaluating bedded mineral deposits . A mathematical proof and examples are given to show that the unweighted and weighted assay averages are equivalent when there is no correlation between assay value and sample interval length but that these averages are different when there is correlation between assay value and sample interval length . The amount of this difference between estimates is a function of the degree of correlation . One set of sample and assay data , based on 11 stratigraphic sections of the Phosphoria formation in Idaho , indicates that the relationship between the amount of difference between estimates and the correlation factor is approximately linear . If this correlation relationship can be established , within acceptable limits of precision , as a consistent attribute of deposits , the estimate of weighted average grade of ore could be predicted directly from the unweighted estimate of grade of ore by using the relationship as a prediction factor . Randomness tests on the sample and assay data from the Phosphoria formation , using the mean - square - successive - difference method , indicate that correlation between assay value and sample interval length ( each sample interval length represents an individual bed or stratum of the formation ) , apparently has little effect on the independence between successive assays , between successive sample interval lengths , and between the products of assays and sample interval lengths . Therefore , these data can be analyzed statistically as long as the original sample sections have been selected at random for sampling .

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 Thomas C. Atchison, Joseph M. Pugliese

Six explosives were compared by measuring their strain- producing abilities in limestone . Peak strain , e , varied with scaled distance , R/Ro , according to the following equation : € = Kc (R /R 。)- ". The distance exponent , n , was a constant of the rock and did not depend upon explosive . The strain intercept , Ke , increased with increasing detonation pressure of the explosive . The strain intercept also depended upon the explosive- to - rock impedance ratio . For impedance ratios from 0.53 to 1.38 , the strain intercept was approximately proportional to the medium stress , Pn , as calculated from the explosive detonation pressure , P , and the explosive - torock impedence ratio , Z , by the simple elastic theory relation : P = 2P / ( 1 + Z ) . PD However , the data indicated that , at lower values of impedance ratio , the strain intercept is relatively larger than would be expected from the simple elastic theory . The results presented provide a simple method for predicting the relative effectiveness of different explosives in breaking limestone from the detonation pressures and characteristic impedances of the explosives .

Jan 1, 1964

By W. J. Boone, Will E. DeVaney, Lowell Stroud

This report is the fifth in a series presenting equilibrium vapor - liquid data for helium- bearing natural gases . It covers a 0.41 - mole - percent - helium natural gas that may be processed in the Department of the Interior's longrange helium conservation program . A Bureau of Mines phase equilibrium apparatus was used to obtain 139 samples of equilibrium vapor and liquid phases at 85 experimental conditions at temperatures from 0 ° to -299 ° F and at pressures from 100 to 500 psia . An appendix covers phase data at 100 , 200 , and 300 psia and at temperatures from -125 ° to -275 ° F for the dehydrated gas containing its original concentration ( 0.2 mole - percent ) of carbon dioxide , and the effect of a preliminary hydrocarbon trap upon subsequent vapor - liquid compositions .

Jan 1, 1964

By R. R. Allen

Gieseler plastometer tests were performed on eight western coking coals at retort - immersion depths ranging from 2 to 3-3 /4 inches (measured to the center of the coal charge ) . Increased maximum fluidities were associated with greater retort - immersion depths , the most pronounced increases being observed on highly swelling coals when tested at 3-3 /4 inches . The maximum fluidity of one of these coals when tested at 3-3 /4 inches was 146 percent greater than that observed at 24 inches . Retort - immersion depth had no significant effect on the temperatures of initial softening , fusion , maximum fluidity , end of fusion , and solidification .

Jan 1, 1964

By William R. Wayment, David E. Nicholson

The Bureau of Mines studied some physical properties of hydraulic backfills and their paramount characteristics , and made preliminary attempts to compact this type of material . The in- place density of hydraulic backfills affects the properties of strength , consolidation , and water percolation . Dense fills give better support than loose fills . In - place density properties themselves are affected by grain size , grain size distribution , and the particular conditions of sedimentation in a stope ( the amount of work the slurry water does to compact the material ) . Field sampling of in - place densities of fills presently used in four different mines and laboratory and underground compaction tests using a standard concrete vibrator show that the initial in - place density of the cohesionless fill material tested can be significantly increased by vibratory compaction .

Jan 1, 1964

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

Batch and continuous - circuit flotation , leaching , precipitation , and electrodeposition studies were made by the Bureau of Mines to determine optimum conditions for treatment of complex mercury - antimony sulfide and mercury- arsenic sulfide ores and concentrates . On the Red Devil ore sample over 95 percent of both the mercury and antimony sulfides were recovered in a flotation concentrate containing 35.6 percent mercury and 21.0 percent antimony . By selective flotation a mercury concentrate containing 71.0 percent mercury and 2.9 percent antimony was obtained with a mercury recovery of 90.4 percent . Leaching results show that , with 150 grams per liter of sodium sulfide and 50 grams per liter of sodium hydroxide , 95 to 99 percent of the mercury , antimony , and arsenic sulfides could be extracted from the concentrates treated . Sodium hydroxide reagent consumption was based on the sulfides generated in the dissolution of the sulfide minerals and on the method of metal recovery used . Selective leaching of the antimony and arsenic sulfides with potassium sulfide dissolved more than 95 percent of either of these two sulfides and 0.5 to 5 percent of the mercury sulfide present . Methods for recovering mercury and antimony from solution were electrodeposition of mercury followed by electrodeposition of antimony , aluminum precipitation of both mercury and antimony , or antimony precipitation of mercury followed by antimony electrodeposition . The method used in recovering the mercury depended on the mercury- antimony content of the solution being treated .Batch and continuous - circuit flotation , leaching , precipitation , and electrodeposition studies were made by the Bureau of Mines to determine optimum conditions for treatment of complex mercury - antimony sulfide and mercury- arsenic sulfide ores and concentrates . On the Red Devil ore sample over 95 percent of both the mercury and antimony sulfides were recovered in a flotation concentrate containing 35.6 percent mercury and 21.0 percent antimony . By selective flotation a mercury concentrate containing 71.0 percent mercury and 2.9 percent antimony was obtained with a mercury recovery of 90.4 percent . Leaching results show that , with 150 grams per liter of sodium sulfide and 50 grams per liter of sodium hydroxide , 95 to 99 percent of the mercury , antimony , and arsenic sulfides could be extracted from the concentrates treated . Sodium hydroxide reagent consumption was based on the sulfides generated in the dissolution of the sulfide minerals and on the method of metal recovery used . Selective leaching of the antimony and arsenic sulfides with potassium sulfide dissolved more than 95 percent of either of these two sulfides and 0.5 to 5 percent of the mercury sulfide present . Methods for recovering mercury and antimony from solution were electrodeposition of mercury followed by electrodeposition of antimony , aluminum precipitation of both mercury and antimony , or antimony precipitation of mercury followed by antimony electrodeposition . The method used in recovering the mercury depended on the mercury- antimony content of the solution being treated .

Jan 1, 1964

By A. L. Service, C. C. Popoff

Phosphate deposits in Montana , Idaho , Wyoming , and Utah are important factors in the mineral , agricultural , and industrial economy in the western part of the Nation . This report presents background information , including geology , mining , beneficiation , processing , resources , and economics , assembled to provide a comprehensive introduction to a series of four area reports . About 20 percent of the Nation's phosphate is produced from the Western field where there were 6 surface and 9 underground mines in operation in 1963 . This region also has an estimated 58 percent of the Nation's phosphate reserves , and continuing development is assured by these abundant resources and an increasing demand for phosphate products . Long range forecasts indicate that the United States will continue to use increasing amounts of both agricultural and industrial phosphate products . Beneficiation has become an important part of the phosphate processing industry , and two flotation plants and several washing plants were in operation in 1963. Recent studies by the Bureau of Mines Metallurgy Research Center , Albany , Oreg . , have been directed toward developing flotation processes applicable to treatment of marginal phosphate rock . Other Bureau of Mines research is being directed toward improved methods of ore recovery , ground control , and mining .

Jan 1, 1964

By K. E. Tame

An alkaline leaching procedure for recovering uranium from a submarginal 0.1 percent Ug Og calcareous carnotite ore from the Shiprock , N. Mex . , area was investigated . A recovery of 72 percent of the uranium was attained in a preliminary test embodying the commonly accepted practice of ( 1 ) alkaline leaching at 90° C , ( 2 ) multiple stage filtration and washing for recovery of a clear pregnant solution , and ( 3 ) caustic precipitation of uranium as sodium diuranate , with recycle of the barren solution to the leaching and washing circuits . Ion exchange resins were used in a second , less orthodox test that comprised ( 1 ) sodium carbonate leaching of minus 10- mesh ore at 90 ° C to dissolve the uranium , ( 2 ) filtration to recover the leaching reagent for reuse , (3 ) recovery of the uranium- bearing solution in the filter cake as a pregnant slime slurry by repulping of the filter cake followed by a sand- slime separation and countercurrent decantation (CCD ) washing for rejection of the sand fraction , (4 ) recovery of the dissolved uranium from the pregnant slime slurry by resin- in- pulp (RIP ) , ( 5 ) elution of the uranium from the resin with a solution of ammonium chloride acidified with hydrochloric acid , and (6 ) precipitation of the uranium with ammonia gas . About 83 percent of the uranium was extracted from the ore and 95.5 percent of the dissolved uranium recovered by ion exchange . Improved laboratory results were obtained using the RIP process , but larger scale tests would be necessary for economic evaluation of the two processes .

Jan 1, 1964

By C. E. Armantrout, H. Kato, M. I. Copeland, M. Krug

The investigation of the nickel - gadolinium phase diagram was undertaken to determine the alloying behavior of these two metals . The data from meltingpoint determinations , thermal analyses , metallographic examinations , and X- ray diffraction analyses revealed a phase diagram with three eutectic points and seven intermetallic compounds . Very limited solubility of the phases in each other was observed . The five phases , Ni Gd , Ni , Gd , Ni Gd , Ni, Gd , and NiGd¸ , melted incongruently at about 1,300 ° , 1,270 ° , 1,180 ° , 1,070 ° , and 775 ° C , respectively . Ni Gd and NiGd melted congruently at approximately 1,550 ° and 980 ° C , respectively . Four of the compounds were determined to crystallize in the hexagonal system : Ni Gd , Ni Gd , Ni , Gd , and Ni Gd . Ni Gd was determined to be cubic and NiGd , orthorhombic . The crystal system of NiGd was not determined . The eutectic points occurred at 13 , 67 , and 85 wt pct gadolinium , and the isotherms at 1,290 ° , 890 ° , and 700 ° C , respectively .

Jan 1, 1964