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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 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 1962. In connection with these purchases , the Bureau analyzed 7,114 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, 1963

By Glen C. Ware

The Bureau of Mines determined the factors involved in the corrosion of starting sheets used in the production of electrolytic zinc with the ultimate purpose of adapting zinc starting sheets to commercial practice . Under present practice , zinc is electrodeposited on aluminum cathodes and subsequently stripped for melting . The use of zinc instead of aluminum would eliminate the need to strip the deposit , thereby reducing the cost of handling and melting it , but zinc has not been suitable because it was too vulnerable to the corrosive attack of the electrolyte . Serious attack was found to be limited to the areas of the cathodes situated immediately above the surface of the electrolyte and to re - entrant corners . It was possible to avoid solution - level corrosion by immersing the starting sheets completely , exposing only a relatively heavy suspension member to solution - level attack . Zinc starting sheets could be made as reliable as aluminum and could be continued in residence for periods up to 39 days . Periods as long as a week were feasible under conditions similar to those found in commercial practice . A test of zirconium as a starting - sheet material showed that it promoted corrosion of the deposit to a lesser extent than aluminum and that the deposit adhered less tenaciously . These two properties lend themselves to the development of ways to strip deposits mechanically from zirconium starting sheets . Titanium was unsuitable for use as a starting - sheet material .

Jan 1, 1963

By C. J. Walker, J. S. Miller

This work was done in an attempt to find a simple solution to the problem of simultaneously changing terminal rate and terminal pressure under conditions of unsteady - state flow in porous media . Although the original aim was not realized , a method for encasing a sandstone core that would permit high - pressure ( 200 to 980 psi ) flow tests and the use of electronic equipment to measure pressures at points along the core during unsteady - state gas depletion was found to be feasible . The sandstone core used in this study was from the Bandera formation of Pennsylvanian age , Redfield , Kans . The core , cylindrical in shape with a 3.5 - inch diameter and 6- foot length , had a porosity of 15 percent and a permeability of 9 millidarcys .

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 R. P. Adams, R. A. Beall

The Bureau of Mines developed a method to melt and cast specimens of hafnium- carbon alloy and studied their properties . A rotating - ladle vacuum or inert atmosphere arc furnace was designed , special electrodes and molds were developed , and operating procedures were worked out for casting small shapes . The cast specimens were evaluated according to their carbon content for melting point , density , microhardness , electrical resistivity , and oxidation resistance . Lattice dimensions were determined , and metallographic specimens were prepared . Photomicrographs were taken of specimens containing 2.72 , 5.50 , 6.47 , 9.97 , 12.8 , and 15.7 weight - percent carbon , and their grain structures were compared .

Jan 1, 1963

By R. V. Higgins, A. J. Leighton

A computer program has been devised to calculate the reservoir performance of water floods of complicated well - spacing patterns . The method and program have been tested by calculating the waterflood performance of fivespot patterns using oils of different viscosities and the performance calculations agreed closely with laboratory results . The program on a high - speed digital computer will process the performance prediction in about 1 minute , which is very rapid for a prediction using so much fluid mechanics and nonlinear geometry . The program has been presented in such a way that one may use it as given and save the time required to write and " debug " one of his own . gram processes a complex reservoir analysis , many of the complicated steps are explained in detail , both for the fluid mechanics and the directions for the computer . The subtle features that originally delayed the application of the program to unusual combinations of permeability and viscosity relationships are incorporated and explained

Jan 1, 1963

By T. E. Green, E. F. Spano, W. J. Campbell

A combined ion - exchange X- ray spectrographic method was developed and evaluated for determining trace amounts of cobalt and nickel in high - purity tungsten and tungsten trioxide . The sensitivity for both cobalt and nickel is in the range from 0.2 to 0.5 μg ( 0.04 to 0.1 ppm , based on 5 gram samples ) . Accuracy at the 5 to 20 μg level is ±10 percent of the amount present . Approximately 16 hours elapsed time is required for analysis

Jan 1, 1963

By Michael G. Zabetakis, Aldo L. Furno, Henry E. Perlee

The Bureau of Mines conducted an experimental study with liquid and gaseous hydrogen to determine the hazards associated with the use of liquid hydrogen as an ionizing particle detector in bubble chambers . The glass window , the vacuum chamber , and the vent system were investigated . In addition , a study was made of the detection and ignition of escaping hydrogen and of the available electrical equipment for use in hydrogen atmospheres . Materials such as tempered glass , aluminum , and stainless steel are not penetrated readily by the small fragments formed when fully tempered glass is shattered and propelled by hydrogen at initial pressures up to 100 psig ; long , slender fragments from untempered glass may penetrate thin walls of relatively soft materials such as rubber gaskets and lead . Hydrogen can be vented satisfactorily from a vacuum chamber with a well - designed vent system . However , the rapid leakage of hydrogen into the surrounding air is a serious problem because the available detectors are satisfactory only when the accumulation of hydrogen is slow . Much of the electrical equipment currently available was designed for use in hydrogen- air atmospheres .

Jan 1, 1963

By K. K. Kershner, J. G. Donaldson

This investigation was conducted to obtain data on optimum conditions for chloridizing metal sulfides . Salt- roasting galena at 450° C for 8 hours chloridized 75 percent of the lead ; in an equal time of treatment at 750° C , the process chloridized 42 percent of the zinc in sphalerite . Hydrogen chloride at 500° C completely chloridized galena in 15 minutes , and at 600° C converted all of the zinc in sphalerite to the chloride in 4 hours .

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 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. 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