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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 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 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 Leonard Obert

This report describes an inexpensive triaxial equipment for testing 2-1 / 8- , 4- , and 5-5 / 8 - inch - diameter rock cylinders subjected to loading conditions comparable to those encountered in underground mining . Only minimal specimen preparation is required . The maximum axial load that can be applied is 250,000 lb , which corresponds to an axial stress of 70,000 psi for the 2-1 /8- inch- diameter specimen . The maximum radial pressure that can be applied is the same for each specimen diameter ; namely , 10,000 psi . The mechanical parts in this equipment are relatively easy to machine and fabricate . The cost of all parts , including the 250,000- lb hydraulic press but not including labor costs , was approximately $ 1,000 .

Jan 1, 1963

By P. A. Wasson, M. M. Fine

Roasting research involving small , batch experiments was conducted to explore the use of solid reductants for converting nonmagnetic iron ore to a magnetic type . Three typical Minnesota ores were tested with one or more of the following reductants : Lignite , lignite chars , anthracite , bituminous coal , petroleum coke , peat , and pyrite . Reductive roasting was accomplished in a 3- by 4- inch externally heated rotating drum . Ore and reductant were placed in the drum and heated to a desired temperature , which was maintained for a predetermined period . Recoveries of over 90 percent of the iron in magnetic concentrates were achieved at 650 ° C , using lignite , some lignite chars , a high- volatile bituminous coal , peat , and pyrite . Pyrite is a novel reductant , which is superior to carbonaceous materials other than lignite and some chars .

Jan 1, 1963

By R. L. Grant, R. W. Van Dolah, N. E. Hanna

An experimental investigation was conducted to assay the relation between natural gas concentration and ignitibility of the gallery atmosphere . Both the gas concentration representing maximum ignitibility and the relationship between certain properties of the explosives and their incendivity are discussed . The data show that variation in the natural gas content in the gallery can have a highly significant effect on ignitibility of the gallery atmosphere ; maximum ignitibility of the atmosphere by permissible explosives occurs with approximately 8.1 percent natural gas . The study also shows that incendivity of a permissible explosive cannot be determined only by its detonation velocity , oxygen balance , or ballistic mortar strength . However , for similar type explosives , trends observed indicate that their incendivity increases with detonation velocity or bulk strength . Additionally , for underoxidized explosives studied here , the more negative the oxygen balance the less incendive was the explosive within a class defined by salt content .

Jan 1, 1963

By V. E. Homme, M. M. Wong

Tests were made in reactors ranging from 12 to 30 inches in diameter to develop methods for the preparation of sodium chloride - titanium lower chlorides ( dichloride and trichloride ) melts that contain titanium predominantly in the divalent state . Such melts are desirable as a starting material for the production of titanium metal or as an electrolyte for electrorefining of titanium . Sodium reduction of TiCl with an 18 - hour period of holding the reaction products in the molten state produced melts that contained titanium lower chlorides in TiCl₂ - to - TiCl , molar ratio of approximately 8 to 1. Sodium reduction of TiCl in a reactor with a shielded pipe weir , that required no melt -holding period , produced melts with a TiCl₂ - toTiCl , molar ratio as low as 4 to 1 . Reduction of TiCl4 with scrap titanium metal in molten sodium chloride produced relatively pure melts containing about 27 percent titanium in a Ticl₂ - to - Ticl , molar ratio of approximately 4 to 1 .

Jan 1, 1964

By Charles J. Stehlik

This report deals with the changing behavior of mine roof bolt and roof rock as a result of repetitious production blasting . Observations were made in the upper shale production headings at the White Pine Copper Co. room and pillar mine , White Pine , Mich . Roof bolt compression pads and a stratascope were used in the investigations , which were carried out in three separate test sites in which nearly identical procedure produced comparative , repetitive , and anomalous observations . Results indicate roof bolt tension change and roof quality deterioration anomalies were coincident with blasting . The hypothesized cause of the anomalies is a seismic shock generated by the blasts .

Jan 1, 1964

By C. A. Pearson, W. D. Dietzman, M. E. Hawkins

Results of chemical analyses and electrical resistivity measurements of 422 samples of oilfield brines from 120 east Texas fields in Railroad Commission of Texas Districts 5 and 6 are presented in tabular form . These samples represent water from all of the major petroleum- productive formations in the area . Water analyses and electrical resistivity data , when fully utilized by proper study techniques , are useful tools in the solution of many engineering problems such as detection of well leaks , identification of water sources , and interpretation of electrical well logs . In the area included in this study , these representative data should facilitate the solution of problems in which water analysis and water resistivity are factors .

Jan 1, 1964

By W. P. Haynes, A. J. Youngblood, J. J. Demeter

Synthesis of high - Btu gas , using the Fischer - Tropsch reaction was investigated in a tube - wall reactor of 2 - inch steel . The catalyst was carbonexpanded iron ( CEI ) , formed on the walls of a steel reactor by exposing the reactor to 1H₂ + 100 synthesis gas under certain conditions . Advantages to be gained from successful development of the CEI - coated tube- wall reactor are elimination of catalyst plant and catalyst handling and charging operations , high- temperature operation , and a relatively low- cost , reactor -heat recovery system . In one test ( TW- 8 ) in which the reactor was filled with CEI , the reactor was operated for 1,910 hours before the test was stopped because of excessive pressure drop caused by carbon deposition . The pressure drop was satisfactory for 1,000 hours of operation at an hourly space velocity of 300 , but it increased rapidly at space velocities of 600 and 1,000 . When operated at a space velocity of 300 , with a ratio of 1 to 1 recycle at 534 ° C , a conversion of 72 percent of the 3H + 100 synthesis gas was achieved . The product gas had a heating value of about 610 Btu per cubic foot and could be suitably upgraded to 900 - Btu gas by subsequent use of a nickel catalyst . CEI did not operate effectively as a film catalyst under conditions of generation tried in this study . Generally , operation of the 2 - inch reactor with CEI catalyst was unsatisfactory because of poor reproducibility of the activation step and poor temperature control resulting in high- operating temperatures and eventual plugging of the reactor . Tests using CEI in fixed , packed beds suggest that the most likely application for CEI in producing high - Btu gas would be a moving - bed reactor , where sufficient bed movement and heat removal are provided to prevent plugging .

Jan 1, 1964

By D. E. Redmon

Linear programing provides a mathematical technique by which activities can be planned in such a way that an optimal result is obtained. Routine applications of linear programing require only a knowledge of algebra. However, a complete understanding of the fundamentals of linear programing requires a knowledge of advanced mathematics. The purpose of this publication is clarification of terminology and illustration of applications in comparatively simple mining problems. Two mining situations are considered: Mine stopes from which ore is to be produced at a minimum production cost; also, uranium mines from which ore is transported to one mill, a maximum monetary value is desired. The details of data arrangement for solution by linear programing are described and the solutions are presented. Results of these solutions indicate successful applications of linear programing to mine production scheduling.

Jan 1, 1964

By F. E. Block, T. T. Campbell, D. Z. Hobbs

Several methods were investigated for the preparation of high- purity elemental boron in an attempt to develop a feasible process for producing boron on a large scale . In the work described in this report , the metal was prepared by metering boron trichloride gas into a crucible containing molten metal reductants . It was necessary to remove reaction byproducts by acid and aqueous leaching . Magnesium and sodium were tested as reductants , but best results were achieved using lithium or zinc as reductants . Contaminants originating from the materials of construction were the chief impurities in boron made by this method . Impurities ranged from 0.5 to 5.0 percent . Impure boron ( 85 to 90 percent ) was also prepared by the magnesium reduction of boron trioxide in a thermite - type reaction . This product contained magnesium as the chief contaminant . Impure boron made in this way could be upgraded by fusing with potassium fluoborate or potassium acid fluoride . After acid leaching the fusion cake , a product containing 95 to 97 percent boron was obtained . Analytical techniques for accurate determination of impurities in elemental boron are a major problem , requiring solution before a valid comparison can be made of the quality of boron prepared by these various methods .

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 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 M. M. Wong, J. E. Klosterman

Scrap beryllium chips ( nominally 96 to 97 percent Be ) were electrore fined in a prototype cell with 408 lb of electrolyte composed of 52.4 mole - percent LiCl , 36.3 mole - percent KC1 , and 11.3 mole - percent BeCl2 . The cell temperature was 500 ° C. In a typical 10-3 /4 - hour deposition cycle , 0.415 pound of metal was produced ; the metal contained impurities in parts per million as follows : C , 700 ; 0 , 610 ; Al , 34 ; Ca , 32 ; Cu , 20 ; Fe , 25 ; Mg , 9 ; and Mn , 23 . Operation of the prototype cell for 2 years demonstrated that adapting the electrorefining process to an enlarged scale of operation presented few difficulties in mechanical functions , maintenance of optimum operating conditions , and control of product purity . After the spent anode feed was leached in a 5 - percent nitric acid solution and the fine - sized particles were removed , it was recycled in some tests . The metal produced was somewhat higher in impurities than metal from the fresh scrap chips .

Jan 1, 1964

By F. R. Cattoir, R. E. Cumings

Columbium metal was electrorefined in a fused - salt electrolyte . Excellent results were obtained in lowering the impurity content in a 94 - percent columbium anode feed material to produce a 99.8- percent - pure metal . The reductions of the major impurities follow : Oxygen from 19,800 to 500 ppm , carbon from 9,700 to 25 ppm , iron from 9,200 to 630 ppm , nitrogen from 2,100 to 90 ppm , and silicon from 750 ppm to not detected . Columbium with a purity of 99.9 percent was produced from 99.5- and 99.8 - percent grades of columbium. The investigation was devoted to the evaluation of a fused - fluoride - salt electrolyte ( KF - NaF- K₂ CbF, ) for electrorefining columbium. The effects of the columbium concentration and the voltage upon the product's purity were investigated . The effect on the cathode current efficiency of ampere - hours of deposition and the formation of a dual valence state of the columbium was also investigated .

Jan 1, 1964

By R. L. Hopkins, H. T. Rall

A continuous method has been developed for preparing thiolacetic acid . Acetic anhydride and hydrogen sulfide are passed concurrently over an amine ion- exchange resin , under 20 - psi pressure . The thiolacetic acid , a product of the reaction , is flashed continuously from the crude reaction mixture and is purified by fractional distillation . The yield of thiolacetic acid is in excess of 80 percent based on the acetic anhydride charged . INTRODUCTION In the synthesis of reference compounds needed in the identification of sulfur compounds in petroleum , thiolacetic acid has become an important reagent because of its use in the synthesis of thiols by addition to appropriate olefins : R - CH = CH₂ + CH3 - COSH R- CH2 - CH2 - S - COCH R - CH2 - CH₂ - SH + CH3COONa NaOH (1 ) The commonly used procedures for its preparation , as described by Clark and Hartman (1 )4 and by Ellingboe (2 ) , are based on the batchwise reaction of acetic anhydride with hydrogen sulfide :

Jan 1, 1964

By Louis A. Panek, John A. Stock

A flat slot is created in rock to cause stress relief effects in a pair of hydraulic borehole pressure cells (previously installed in drill holes above and below the slot ) , which act as sensing devices . This relief is annulled by repressuring the slot by means of a flat hydraulic cell . The slot pressure at annulment is taken to be the existing ground stress at right angles to the plane of the slot . A number of trial installations in the rib of a mine drift showed that for a valid determination of ground stress the sensing devices that respond to relief and repressuring must be within a specified zone close to the pressure transmitter ; otherwise the indicated ground stress may be excessive . By using an additional pair of borehole pressure cells , installed a few feet away , the existing rock stress can be redetermined at intervals , irrespective of a change of stress intensity subsequent to the initial installation . Based on these findings , equipment and procedures have been developed that make possible the installation and operation of a permanent rock stress monitoring station for observing mining - induced stress changes . The station consists of a 12 - in - wide hydraulic pressure cell cemented in a flat slot and four 2- by 8 - in flat hydraulic pressure cells in nearby drill holes . All drilling for the installation can be done with an air leg drill and conventional bits . Once the installation is completed , all required information is obtained by Bourdon pressure gage readings . The apparatus is simple , relatively inexpensive , and reliable under operating conditions in a wet mine . Unlike most methods of rock stress determination , this scheme permits periodic remeasurement of absolute rock pressure over several years , without additional drilling or instrumentation . Similar to other flat slot procedures , stress measurements are obtained without making auxiliary tests to determine elastic

Jan 1, 1964

By David W. Wisecarver

This report describes a tool to engage and/or place a Bureau of Mines type gage to measure borehole deformation in a horizontal , 1½ - inch - diameter , stress relief borehole . The tool was successfully used at a borehole depth of 105 feet . Practical usage up to borehole depths of 200 feet might be realized . The tool was designed to work inside EX- size ( 1½ - inch ID ) diamond - drill drive casing used as drill rod and through which the deformation gage is guided into an EX- size stress relief borehole . Through laboratory experiments it was found that by exercising a reasonable amount of care the deformation gage could be placed at a point within a ± .01 foot distance of a predetermined depth in a horizontal EX- size hole and that the deformation measuring piston or plunger of the gage could be oriented in the borehole within 0.5 ° of a preselected angle of orientation in a vertical plane .

Jan 1, 1964

By R. W. Hiteshue, C. O. Hawk, H. H. Ginsberg, M. D. Schlesinger

The Bureau of Mines studied single - step catalytic vapor - phase hydrogenation of oils derived from coal and oil shale . Treatment of middle oil , from hydrogenation of bituminous coal , gave good yields of gasoline with a German - made molybdenum- zinc - chromium catalyst . The Bureau also achieved good results with duplicates of this catalyst made from domestic raw materials . In one set of experiments with the German catalyst , 38 to 52 wt pct of feed was converted to gasoline . The total liquid product was 91 to 98 wt pct of the feed . Not all this gasoline can be claimed as production , however , because about 20 pct of the feed was in the gasoline range , and part of it undoubtedly survived the hydrocracking treatment . Hydrogenation of crude shale oil in the presence of cobalt molybdate catalyst produced a total liquid product of 89 wt pct of feed . The hydrogenation converted 27 wt pct of feed to gasoline and 44 wt pct of feed to diesel fuel . The remaining liquid product , 18 wt pct of feed , was residue boiling above diesel fuel . The gasoline was of poor quality , with an octane number of 39.1 . The overall product seemed a suitable feed stock for a conventional refining operation . Coker distillate hydrogenation , using a cobalt molybdate catalyst , gave a total liquid product of 97 vol pct of feed ; of this product 60 vol pct was jet fuel and 40 vol pct was diesel fuel . High nitrogen and sulfur in all three of these raw materials severely poison the usual refining catalysts . Thus , the common objective in these

Jan 1, 1964