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By Henry E. Blake

Defluorination studies on refractory fluoride - bearing compounds and minerals , particularly on partly defluorinated residues from high - temperature pyrohydrolysis , required a dependable and reasonably accurate analyticalcontrol method for the analysis of fluorine . The difficulty in liberating fluorine from the fluorides of metallic elements such as aluminum, zirconium , and rare earths by steam- distillation can be largely overcome if the distillation is made from a sulfuric - phosphoric acid solution of a sodium carbonate fusion of the sample material and if the distillation temperature is maintained at about 155 ° C. The data presented in this paper show that liberation of fluorine by this method is more complete and proceeds more rapidly than by usual distillations from perchloric or sulfuric acid alone or a mixture of phosphoric and perchloric acids . Fluorine in amounts ranging up to about 140 mg can be recovered by collecting only about 300 ml of distillate . Determination of fluoride in the distillate is made by the usual thorium nitrate titration .

Jan 1, 1963

By W. E. Lamont, R. E. Perry, I. L. Feld

The Bureau of Mines conducted research to determine the conditions required to sinter a pyrrhotite calcine into a product suitable for iron blast furnace feed . The calcine , a fine - grained iron oxide produced by roasting sulfide flotation concentrate , analyzed about 60 percent iron and 1 percent sulfur . Sintering of the calcine without prior pelletization was not successful whereas firing of preformed calcine charges yielded acceptable sinter products . Batch tests were made to study the effect of the following variables on the sinter quality : Size of green pellets in the charge , quantity and type of internal carbonaceous fuel used , depth of sinter bed , moisture content of the charge , flux additions , and binder additions . The batch and continuous sinter tests showed that minus 1 / 4 - inch pellets prepared from a mixture of the calcine , coke , dolomite , and water gave sinter cakes analyzing 57 to 61 percent iron and 0.05 to 0.02 percent sulfur .

Dec 1, 1963

By B. B. Letson, D. F. Smith, T. E. Gardner, A. R. Taylor

Low- temperature heat capacities of strontium chloride (7° - 300° K) and strontium fluoride ( 11 ° - 300 ° K) were measured with an adiabatic calorimeter . Smooth values of heat capacity , entropy , enthalpy function , and free - energy function were calculated from the heat - capacity data . The smooth values are reported at 10 ° K intervals and at 273.15 ° and 298.15 ° K.

Jan 1, 1963

By E. C. Perkins, R. S. Lang, D. M. Taylor, H. Dolezal

The amenability of titaniferous slags and domestic mineral concentrates to chlorination was determined in a 6 - inch diameter fluidized bed chlorinator . Ilmenites from Valley County , Idaho ; Aiken , S.C ,; Trail Ridge , Fla .; and MacIntyre , N.Y .; and a titaniferous magnetite from Iron Mountain , Wyo . , were used in preparing the slags . The domestic minerals tested were an ilmenite concentrate from Valley County , Idaho , and a rutile concentrate from Magnet Cove , Ark . A high - grade Australian rutile was used as a standard for comparison . The impurity content of the slags and minerals tested , which was the most critical factor affecting their performance , was dependent on the geographical source of the material . All of the materials tested were amenable to chlorination in a fluidized bed although some required special operating conditions . Titanium extractions and chlorine utilization were over 90 percent for most of the slags and the Australian rutile . The Valley County , Idaho , ilmenite performed well in the reactor despite its 34 percent iron content .

Jan 1, 1963

By R. A. Friedel, J. L. Shultz, A. G. Sharkey

The purpose of this investigation was to study the primary materials associated with the coal structure . Mass spectrometric techniques can be useful in studying the chemical structure of coal and various high- molecularweight materials derived from coal . Investigations of pyrolysis products and extracts of coal , and also whole coal , showed : 1. Aromatic hydrocarbons obtained by the vacuum pyrolysis of coal below 300 ° C possibly were sorbed material rather than decomposition products . 2 . 2 . Thirteen structural types having molecular weights from 78 to 400 were identified in pyridine extracts constituting one - quarter or more of the coal by weight . 3. Material extracted at room temperature with a methanol - benzene solvent and a vacuum pyrolysis condensate obtained at 450 ° C contain similar components . The extract and the condensate have approximately the same average molecular weights ( 200-300 ) . 4. Material extracted from coal at room temperature is altered even by mild thermal treatment . 5. Changes in various alkyl series occurring in thermally treated coal extracts can be followed quantitatively . 6. Similarities in the spectra of coal and graphite were indicated in an investigation using a mass spectrometer equipped with a spark source . Determinations on a coal - ash sample by this technique showed good agreement with data obtained by emission spectroscopy .

Jan 1, 1963

By R. H. Storch, D. C. Holt

During reconnaissance investigations of more than 300 stream areas in Idaho to determine the potential value of ilmenite in black - sand placer deposits 46 deposits were explored by churn drilling , trenching , test pitting , or shafting . The component mineral content and total black - sand content were determined for more than 8,690 reconnaissance and exploration samples . Data compiled during the investigation indicate a good potential for large , low- grade deposits containing ilmenite , monazite , columbite , euxenite , uranothorite , and other radioactive black minerals and accessory black - sand minerals . The data also indicate most deposits will be economic only if several component minerals can be recovered as coproducts .

Jan 1, 1963

By F. E. Brantley, D. A. Martin

Synthetic zeolites were tried as selective adsorbents for recovering sulfur dioxide from synthetic gases and gases produced from gypsum decomposition . Initial adsorption tests , using the synthetic gases , indicated that three of these compounds , having sulfur dioxide capacities of up to 29 grams per 100 grams of adsorbent , were satisfactory . Regeneration studies showed that over 90 pct of the sulfur dioxide desorbed from the loaded beds was of sufficient purity for direct liquefaction . However , all zeolites tested lost adsorptive capacity with repeated use . The zeolite determined to be the most promising in the preliminary synthetic gas tests was also evaluated for capability in adsorbing sulfur dioxide from gases produced by the thermal decomposition of gypsum . Despite small amounts of hydrogen sulfide in the gypsum decomposition offgas , good adsorption of sulfur dioxide was attained . The economic practicality of utilizing zeolites for sulfur dioxide removal from industrial gases was not evaluated , but the technical feasibility was demonstrated .

Jan 1, 1963

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

About 95 pct of the beryllium was dissolved from most ore samples by agitation leaching with 600 lb of H2SO4 per ton of ore for 24 hours at 65 ° C and 35 pct solids . Leach slurries generally were viscous , and the limiting pulp density for thorough mixing was about 35 pct solids . Settling of the leached pulp required 0.6 to 0.8 lb of a polyacrylic flocculant per ton of ore leached with 600 lb of H2SO4 per ton , whereas ore leached with 800 lb of H2SO4 per ton required only 0.2 to 0.3 lb of flocculant per ton . Terminal densities of the settled pulps were about 28 and 35 pct solids , respectively , from leaches using 600 and 800 lb of H2SO4 per ton . Vacuum filtration of settled pulps at 15 in . Hg resulted in a filter cake containing 50 to 59 pct solids . Roasting the ore at 500 ° C before leaching increased the limiting pulp density for effective mixing to 50 pct solids . Acid requirements , however , were not diminished , although leaching roasted ore with 600 lb of H2SO4 per ton resulted in densification of settled pulps to about 40 pct solids . Filter cake from leaching preroasted ore contained about 20 pct less water than that from unroasted ore .

Jan 1, 1963

By D. Bienstock, R. C. Kurtzrock, E. R. Bauer, J. H. Field

To remove hydrocarbons and carbon monoxide in automotive exhaust by oxidation , a catalyst of 4.2 percent Uз Og , 1.7 percent Cr₂ 0 , and 1.7 percent CuO supported on 1 /8 - inch y- alumina spheres was tested in a reactor in place of the muffler of a 1 / 2 - ton truck . Tests were made with both nonleaded and leaded gasolines . With the engine at operating temperature , tests were made with the engine idling and with the vehicle cruising at 30 mph . Auxiliary air was added to maintain an oxygen concentration of 3 to 4 percent in the gas leaving the catalytic reactor . The vehicle was operated for 83 hours (about 60 percent of the time with the engine idling ) and 525 miles with nonleaded gasoline . Conversions of 98 percent of the hydrocarbons and 100 percent of the carbon monoxide were achieved with the engine idling and with 7,000 ppm carbon atoms and 4- percent carbon monoxide in the feed to the reactor . Hydrocarbon conversions of 75 percent were obtained at cruising speeds of 30 mph with a feed of 1,700 ppm carbon atoms ; the carbon monoxide concentration was less than 0.3 percent in the feed and was unchanged in passage through the reactor . Identical activity was obtained initially in switching to a gasoline containing 1.9 ml tetraethyl lead (TEL) per gallon . However, there was a gradual loss in activity thereafter . Conversions in tests with the engine idling about 50 percent of the time , had decreased by 23 percent for the hydrocarbons and by 25 percent for the carbon monoxide from their initial values after 122 hours and 1,300 miles of operation with leaded gasoline . The levels of radioactive materials in the exhaust of the reactor and the radiation in the vehicle were negligible .

Jan 1, 1963

By W. E. Bruce, James Paone

Drillability or a measure of drilling performance has been based on ( 1 ) hardness and toughness of rocks , ( 2 ) power input to the drill compared with total volume of hole , and ( 3 ) penetration related to resistive forces of rock on the applied penetrative forces . An analysis of some representative previous work is made . Experimental drillability curves from AX- size diamond core bit performance in eight different rocks ranging from dense hard taconite to soft limestones are presented . Results show that in small bore diamond drilling , compressive strength and possibly other rock properties may be a useful parameter in predicting drilling rates .

Jan 1, 1963

By J. H. Holden, C. C. Shale, G. R. Strimbeck, W. S. Bowie

Electrical characteristics are presented for air in a 2 - inch pipe - type electrostatic precipitator operating under dynamic conditions at temperatures of 600 ° to 1,500 ° F and pressures of 0 to 80 psig using a negative discharge electrode . Results of this one - geometry study show that current - voltage relationships are a function of air pressure and temperature and indicate that precipitators can be used at any temperature through about 1,350 ° F over the full range of pressure . Corona starting voltage and sparkover voltage vary directly with pressure and inversely with temperature . At temperatures above 1,350 ° F use of precipitators may be limited to operations at pressures somewhat above atmospheric pressure . Theoretical derivations are presented that relate the effect of gas density on corona starting voltage and the effect of ion mobility on corona current . Deviation from the theory is noted at high current levels . Theoretical discussion is presented to explain the apparent electrical limitations for use of precipitators at high temperature , low gas density , and high corona currents , conditions at which calculated ionic velocities are extremely high . Experimental results are interpreted in terms of the theory presented . 1,500 ° F thermal ionization does not appear to be a critical factor .

Jan 1, 1963

By Martin H. Stanczyk, I. L. Feld

Continuous open - circuit attrition grinding of a coarse commercial kaolin to produce paper - coating clay , which must have a particle size analysis of 70 percent or more minus 2 - micron equivalent spherical diameter ( esd ) , was studied by the Bureau . The coarse clay , containing about 11 percent minus 2 -micron esd material , was ground in a 10 - inch- diameter attrition grinder using continuous single- and multiple - stage grinding circuits . The clay feed rates varied from 10 to 480 pounds per hour . In some tests , the influence of varying loads of sand grinding media on particle size reduction was studied . Batch grinding tests also were made for comparative purposes . Multiple- stage grinding gave better results than single - stage treatment when equivalent raw clay feed rates were used . In the best test made , a product containing about 80 percent minus 2 - micron esd material was obtained when grinding 60 pounds of raw clay per hour using a three - stage grinding circuit . Power consumption in the test was about 318 kilowatt -hours per ton of clay treated or 475 kilowatt - hours per ton of minus 2 - micron esd material produced .

Jan 1, 1963

By Robert M. Becker

This investigation (in five parts) extends the theory of sample reliability from a sample consisting of a fixed number of items to a sample consisting of a fixed amount of items. Examples of a fixed amount of items per sample are samples consisting of a fixed weight or a fixed volume of unequal size particles. The extension of the theory is confirmed by experimental laboratory sampling using standard procedures. The probability distribution functions (the binomial, hypergeometric, multinomial, generalized hypergeometric, and those here called the compound binomial and compound multimomial functions) are developed from fundamentals. Their distributions are generalized to include some measured characteristic of the items. Infinite population moments are derived from moment-generating functions, and finite population moments are developed from corresponding infinite population moments using a newly defined mathematical operation. The first three experimental moments in laboratory sampling to given weights of particles are compared with the theoretical moments of their corresponding compound mult.inomial distributions. The agreement is striking. The study is divided into five parts. Part 1 deals with probability or random sampling to n items and with all sampling to n items per sample from some one probability distribution. This is the area of sampling covered by well-known theory. Accordingly, the procedures may be different but many of the results are well known.

Dec 1, 1964

By John J. Mulligan

Coalbeds were discovered in outcroppings of the Beacon group of sediments on the north end of the Willett Range ( altitude 77 ° 11 ' S , longitude 160 ° 20 ' E ) , Victoria Land , Antarctica , in December 1960 during an investigation undertaken as part of the U.S. Antarctic Research Program under the auspices of the National Science Foundation . Three separate exposures of coal or coaly material were found . Two of the exposures contain , respectively , eight and four beds of hard , compact , finely banded attrital coal ranging in thickness from 8 feet downward to a few inches , and reported to range in rank from mediumvolatile bituminous to semianthracite . The coals are associated with carbonaceous shales containing an abundant assemblage of fossil plants resembling those associated with the Permian coals of Australia and other Gondwana areas . The third exposure , apparently somewhat higher in the stratigraphic sequence , contains only coaly plant fragments scattered through a thin conglomerate and overlying sandstones . A sandstone bed that overlies these coal - bearing sandstones contains abundant logs and fragments of silicified wood . Preservation of features is poor , but one segment of a silicified stem suggests comparison with Rhexoxylon , a gymnospermous tree that usually is considered indicative of Triassic age . The Beacon sediments in this area have been invaded , broken , and uplifted by a massive series of diabase sills and dikes greater in volume than the intruded sediments . The heat emitted by these intrusives must have advanced the metamorphic development of the coals . However , there is no evidence of alteration to graphite , and coal found in direct contact with a diabase sill contains no vesicles or other usual evidences of natural coking . Either the pressure of overlying rocks inhibited the development of coke , or the coals had been metamorphosed beyond the coke forming stage before the igneous intrusion .

Jan 1, 1963

By Wilbur I. Duvall, Thomas C. Atchison, Joseph M. Pugliese

Short cylindrical charges were detonated in drill holes in rock to determine the effect that decoupling ( defined as the ratio of the radius of the hole to the radius of the charge ) has on the strain - generating abilities of explosions in rock . The amplitude and period of the strain pulses produced in the rock were studied as a function of distance , size of charge , and decoupling . The main results of these studies were that , for a given distance and size of charge , the amplitude of the strain pulse decreases as decoupling increases and the period of the strain pulse decreases at first and then increases as decoupling increases . A simplified theory of decoupling is presented that satisfactorily explains the experimental results . The information presented makes it possible to predict the effect of decoupling on explosiongenerated strain pulses in rock and thus helps the explosives user evaluate the effect of decoupling on his blasting .

Jan 1, 1964

By David D. Walker

The purpose of the investigation was to describe and appraise tungsten deposits in Montana . The work supplements previous investigations made by Pattee ( 10 ) and Walker ( 17 ) in selected areas of the State . Scheelite deposits in tactite are the most numerous and most important economically , having accounted for nearly all of the State's tungsten production . Of the 64 deposits examined during the current study , 50 contained scheelite , 11 hubnerite , 2 wolframite , and 1 ferberite . The State's major tungsten production has been from scheelite deposits in Beaverhead County . The report lists , by counties , the type and grade of each deposit . The more important occurrences are accompanied by geological and assay maps .

Jan 1, 1963

By R. V. Lundquist, H. Leitch

Two hydrated calcium aluminates , formed by side reactions in the leaching step and desilication step of the lime- soda sinter process , were investigated to better define their influence on alumina recovery . The two calcium aluminates , Caз [ Al ( OH) 6 ]₂ and зCa0.Al½ 03 · ( 8-12 ) H₂ ) , were prepared and identified by chemical and X- ray analysis . The relative proportions of each of these compounds formed in typical leach solutions at several temperatures were determined . The influence of free lime as a promoter of calcium aluminate formation was also investigated . The formation and precipitation from leach liquors of calcium aluminates contributes to the low alumina recoveries in the process . The presence of carbonate ion in the leach solution suppresses calcium aluminate formation and precipitation and results in higher alumina recovery . Hydrated calcium aluminates are formed in the aging of lime - soda sinters in the normal atmosphere .

Jan 1, 1963

By L. Mark Irwin, R. A. Marsyla

The objective of this laboratory investigation was to develop a mattesmelting process for the recovery of copper from industrial smelter dusts . Experimentation was conducted on three samples of Cottrell precipitator dust from a northern Michigan smelter with variations in the following conditions : Temperature , charge composition , pelletization , and moisture content . Based on chemical analyses of the furnace slags , poorest recovery of copper was effected in smelting dry charges regardless of composition . Some improvement was noted with uniformly moistened charges and still more with pelletized (but dry) mixes , but best results were obtained from smelting moist , self - fluxing pellets . Under favorable conditions , experiments yielded furnace slags with an average copper content of only 0.15 percent , which is well below that of industrial copper reverberatory slags .

Jan 1, 1963

By Alla D. Mah

The energies of combustion of two carbides of tungsten and two carbides of molybdenum were measured , and the corresponding standard heats of combustion were derived . The results are as follows : WC : AH298.15 ( combustion ) = -285,940 ± 250 cal /mole , W₂ C: AH298.15 (combustion ) = -490,660 ± 400 cal /mole , Mo₂ C : AH298.15 ( combustion) = -439,350 ± 600 cal /mole , MoC : AH298.15 ( combustion ) = -269,800 ± 1,000 cal /mole . The combustion heats were combined with the heats of formation of the corresponding metal trioxides and carbon dioxide to obtain the following heats of formation : WC : AH298.15 ( formation ) = -9.6 ± 0.4 kcal /mole , WC: AH298.15 ( formation ) = -6.3 ± 0.6 kcal /mole , Mo₂ C : AH298.15 (formation) = -11.0 ± 0.7 kcal / mole , MoC : AH298.15 (formation ) = -2.4 ± 1.0 kcal /mole . The heats of combustion and formation of MoC are tentative .

Jan 1, 1963

By Robert T. Beckman

The results of a preliminary investigation of compressive strength versus length-diameter (L/D) ratios of potash specimens and the statistical treatment of the data are summarized in this report. The purpose of the study was to evaluate a laboratory method for obtaining estimates of the strength of potash pillars during robbing operations. The specific objectives of this preliminary investigation were to test the method and the reliability (confidence limits) of the data, and to determine the number of additional specimens necessary for given confidence limits. The specimens were taken from three sites at two mines in New Mexico. The statistical analyses included the determination of the confidence limits for the data and the number of additional specimens necessary to obtain confidence limits of ±500 and 100 psi. The testing method was found acceptable, and estimates of the comprehensive strength, within 1500 psi, could be obtained by testing about 110 additional specimens from the three sites. The compressive strength of the specimens tested fits an empirical equation of the type

Dec 1, 1963