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By David Schlain

A small alumina reduction cell with a graphite crucible and boron nitride liner was developed by the Bureau of Mines as the initial phase of a study of the reactions which occur in the reduction of alumina by the Hall-Heroult process. Operating conditions in the cell such as temperature, time, current density, electrolyte composition, and electrode materials may be varied easily. Aluminum was produced in the cell at a current efficiency of about 75 percent and a cell voltage of 2.7 volts. Although the data are not wholly conclusive, the operation of the cell did not appear to be greatly affected by large changes in temperature, electrode spacing, current density, and alumina concentration in the electrolyte.

Jan 1, 1963

By Wilbur I. Duvall

Twelve millisecond delayed blasts in four limestone quarries in Iowa were instrumented with arrays of vertical velocity gages to determine if the direction of propagation through the rock or the method of initiation of the blast had any effect upon the level of vibration. Two gage arrays approximately 90° apart were used to test the effect of direction of propagation. The vibrations from blasts initiated by three methods were recorded. Vibration records from these tests were analyzed for peak particle velocity as a function of distance from the blast. The data are shown to fit a power Law equation. Direction of propagation is shown to affect the value of the exponent n. The effect of charge size per delay interval on the level of vibration is removed from the data by scaling the travel distance by the square root of the charge weight per delay period. The method of initiating the blasts is shown to have a strong effect upon the level of vibration and the spread in the data from one shot to another.

Jan 1, 1963

By Thomas M. Nasiatka

Tests with a high-pressure water jet were conducted in the steeply pitching Roslyn No. 5 bituminous coalbed in the Roslyn No. 9 mine, Roslyn, Wash., to determine the feasibility of extracting coal from pillars and from a solid coal face in development without drilling and blasting. During pillar mining, using a hand-held monitor, the best results were obtained with a 0.150-inch- diameter nozzle, a water pressure of 3,500 psi, and a flow rate of 38.5 gpm.3 The rate of mining and productivity were 0.74 ton per minute and 16.6 tons per man-shift, respectively. During development mining, using a monitor mounted on a roof jack, the best results were obtained with a 0.148-inch-diameter nozzle, a water pressure of 4,500 psi, and a flow rate of 40.0 gpm. In one section of the mine where the coal was relatively hard, the rate .of mining and productivity were 0.10 ton per minute and 5.7 tons per man-shift, respectively in another section of the mine where the coal was relatively soft, the rate of mining and productivity were 0.51 ton per minute and 8.3 tons per man-shift, respectively. The tests showed that hydraulic mining methods were more productive than conventional mining methods in pillar mining. In development the productivity of hydraulic mining depended primarily upon the coal hardness. Compared with conventional methods, hydraulic mining methods were less productive where the coal was relatively hard and equally as productive where the coal was relatively soft.

Jan 1, 1963

By Martin H. Rogoff

The presence of antibiotic materials extractable with polar organic solvents was demonstrated in coals of various ranks. Since these antibiotics occur in low concentrations, 200 pounds of a high-volatile C coal was extracted with acetone at room temperature to obtain sufficient material for detailed study. The biologically active materials in the extract were concentrated by extracting with aqueous sodium hydroxide. The fractions soluble in sodium hydroxide inhibited bacterial cultures when present in concentrations comparable to those at which other antibiotics are active (5 µg/ml). Steam distillation of the extracts did not yield highly active materials, contrary to the finds of other investigators. Mass spectrometry of the extract indicated, mainly, the presence of 6-ring compounds in the region of mass 324 to 392. The predominance of 3-ring aromatic systems found by ultraviolet analysis suggests compounds such as biphenanthryl or similar structures. The activity of the hydroxide- soluble material decreased markedly when the phenolic hydroxyl groups were transformed into trimethylsilyl ethers. Hydrolysis of the ethers yielded a product having the same activity as the original material, which indicates that phenolic compounds are largely responsible for the antibiotic activity observed.

Jan 1, 1963

By D. E. Hirsch, J. W. Davis, Norman G. Foster, F. G. Schwartz

This investigation was undertaken to identify nitrogen , oxygen , and sulfur compounds (polar components ) found in catalytically cracked distillate fuel . It is significant that these compounds concentrate in the sediments and gum that form when the fuel is stored . The polar components were divided in three portions by elution from a chromatographic column filled with alumina . After the hydrocarbons were washed through the column with pentane , a benzene eluted extract was removed followed by an ether eluted extract and then an alcohol desorbed fraction . These extracts were individually distilled in a molecular still and the fractions were analyzed by gas chromatography , mass spectrometry , infrared spectrometry , and elemental and functional analyses . Naphthalene and its homologs , phenanthrene and its homologs , and other compounds such as methyl indene , C₂ quinolines , phenyl indan , and the benzothiophenes , appear in the benzene extracts . Quinolines are the major components of the lower boiling fraction of the ether extract , although carbazoles , acridans , and indoles are present in some concentration . Elemental and functional group analyses of the alcohol fraction indicated 10 percent of the distillate portion was nonhydrocarbon , and in this portion the average molecule contained more than one nonhydrocarbon element . Compounds of such complexity are not well known , and standards for positive identification are limited .

Jan 1, 1963

By L. G. Trudell, J. W. Smith, K. E. Stanfield

Representation of actual oil yields from sections of the Green River formation oil shales by two types of drill - cutting samples was evaluated . Average oil yields of single sets of mud cuttings from hydraulic rotary drilling in Colorado and gas cuttings from pneumatic rotary drilling in Utah were compared statistically with yields of core samples taken from adjacent holes . Oil yields from gas cuttings were identical to oil yields of core samples . Mud cuttings appeared to represent a section of the formation conservatively , the deficiencies increasing with increasing richness of sample . Because a large amount of the oil - yield data currently available for the Green River formation is based on mud- cutting samples , development of a valid correction method by additional testing is needed .

Jan 1, 1963

By Robert E. Meredith, Thomas T. Campbell

An investigation was undertaken to examine the feasibility of employing low- temperature nonaqueous baths for electrodepositing some of the refractory metals of the ferroalloy group . To date , such metals as tungsten , molybdenum , and vanadium have been produced only by high - temperature processes that are technically difficult and sometimes cumbersome in operation . Deposition studies were performed in a wide variety of organic solvents , including amides , ammonia derivatives , ketones , polyhydroxy alcohols , and ethers . Compounds prepared and used as solutes included the chloride and bromide salts of vanadium , tungsten , and molybdenum . Studies were conducted over a temperature range of 20 ° to 200 ° C under inert atmosphere . Conductivity and current potential data were obtained for all baths that contained reasonable solute concentrations . Qualitative solubility data were obtained for compounds of ferroalloy metals in a variety of solvents . In general , all solutes showed low solubility in ethers and ketones but reasonable solubility ( in excess of 20 grams per liter ) in alcohols , amides , and ammonia derivatives . No successful metallic deposits that would encourage further study were obtained with any of the systems that were examined .

Jan 1, 1963

By H. P. Hamlin, W. A. Grosh

Samples of clays , shales , and argillites from 21 locations were subjected to preliminary bench- scale tests for bloating properties , and several samples were tested for ceramic properties . Samples showing favorable bloating properties were further tested in a pilot - plant - scale rotary kiln . Physical characteristics and concrete -making properties of the bloated products were determined . The Decorah shale from one area made a suitable material for a lightweight aggregate ; however , the limestone layers in the formation must be eliminated or the resulting activated lime must be controlled by quenching .

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 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 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 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 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 Donald W. Mitchell, John Nagy

Observations made on coking of coal, deposition of soot, dust transport, flame, violence, and related phenomena following experimental coal-dust explosions are summarized. Data are given on gas explosion pressure, flame length, flame velocity, and variation of these parameters with concentration. Conclusions from these observations are useful in preventing similar occurrences in operating mines and serve as a guide in improving safety.

Dec 1, 1963

By H. A. Dierks, H. B. Link

The purpose of this investigation was to develop a practical feeder apparatus to introduce comparatively large pieces of coal and similar material into a pipeline under pressure in connection with the vertical hydraulic transportation of solids , termed " hydraulic hoisting . " This method of hoisting the precrushed run - of - mine product of an underground mine has been given unusually wide attention abroad and could be of considerable significance to the U.S. mining industry in its search for operating improvements and cost reduction . A lock-hopper assembly was developed after a series of sinking velocity tests were made by dropping anthracite in a column of water . The system functioned reliably as an automatically operated feeder apparatus .

Jan 1, 1964

By A. F. Colombo, D. W. Frommer

Bench- scale tests were made to determine the applicability of flotation as a means of upgrading finished and semifinished magnetic concentrates prepared from reductively roasted iron ores . Both anionic and cationic flotation methods were used to remove siliceous gangue from the magnetic concentrates and produce upgraded products . Seven magnetic concentrates , containing from 6.7 to 13.7 percent SiO2 , were improved by the flotation treatment , yielding final concentrates containing less than 6.0 percent Si02 . Cationic flotation methods were studied on four of the seven samples ; of this group only one sample yielded better results by cationic flotation than by the anionic method .

Jan 1, 1964

By F. D. Everett

Thermoelectric and metal alloying applications have changed the status of tellurium from oversupply to under supply . In a search for new sources of this element in Arizona , Colorado , New Mexico , Utah , and neighboring states , the Bureau of Mines analyzed more than 200 samples and obtained the results of tellurium determinations by private companies on more than 500 samples from a wide variety of mineral - bearing deposits . The About 40 minerals containing tellurium have been reported , mainly tellu- rides of gold , silver , bismuth , mercury , lead , copper , iron , and nickel . minerals usually occur in small quantities and identification in ores is extremely difficult . Samples containing more than 0.1 percent tellurium were taken from the Hilltop and Memphis properties in Dona Ana County , N. Mex . , and the Silver King property in White Pine County , Nev . , where development was chiefly for base metals . The Lone Pine mine in Catron County , N. Mex . , and the Bambolla mine near Moctezuma , Sonora , Mexico are potential sources of native tellurium occurring in small but high- grade pods . Much of the production of tellurium has come as a byproduct of electro- lytic refining of copper and lead- zinc ores in Arizona , Colorado , New Mexico , and Utah . Base -metal ore deposits will continue to be the most important pri- mary source of tellurium , although the concentration in ores is nearly always less than 10 parts per million . Any significant increase in output of tellu- rium probably will be related to production and improved efficiency in smelt- ing and refining base - metal ores .

Jan 1, 1964

By R. Barany

The heat of formation at 298.15 ° K of muscovite was determined by solution calorimetry . The value obtained for the heat of formation from the elements was -1,421.2 ± 1.3 kcal / mole , and the value for the heat of formation from the oxides was -55.9 ± 1.3 kcal /mole .

Jan 1, 1964

By Theodore L. Turner, Joseph H. Swift

A study on a small laboratory scale was made of the use of ammoniacalammonium carbonate for batch leaching Mn from low- grade manganiferous materials ( 6 to 16 pct Mn) obtained from deposits in the southern district of Aroostook County , Maine . These materials were partially reduced at 500 ° to 700 ° C with H₂ or CO and then leached with solutions of NH and CO₂ dissolved in water . Extraction of 80 to 90 pct of the Mn was obtained from some sample materials , but 10 to 34 pct of the iron was also extracted . Material from the Littleton Ridge deposit contained manganese intimately associated with Fe , a condition which contributed to difficulties in obtaining a commercially acceptable product . Extensive investigations of the leach and reduction processes with various mixtures of H₂ and water vapor , and CO and CO₂ , failed to disclose a set of conditions for selectively leaching the manganese . Finely divided metallic Fe was probably produced during the reduction steps so that Fe was leached with the Mn in the subsequent extractions .

Jan 1, 1964