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By W. P. Haynes, J. W. Mulvihill, G. B. Taylor, S. Katell

Capital and operating costs have been estimated for separating methane and hydrogen in gas - separating plants designed to produce 90 million scf per day of product gas containing a minimum of 90 percent methane . After a preliminary literature review of various separation techniques , three different processes --moving - bed adsorption using active carbon , oil absorption , and liquefaction -- were chosen for the cost estimates . Three different methane feed gas concentrations , 5 , 20 , and 50 percent ( cases 1 , 2 , and 3 , respectively ) , were chosen as representative methane concentrations for the separation estimates . Capital and operating costs were lowest for the moving - bed adsorption process in all three cases investigated . Operating costs declined from $ 0.24 to $ 0.06 per 1,000 cu ft of product gas , and capital costs declined from $47,490,800 to $7,411,200 as the percentage of methane in the feed gas increased from 5 to 50 percent .

Jan 1, 1964

By John Ward Smith, Neil B. Young

Shale specific - gravity to oil - yield relationships were developed for black shales of the New Albany Formation of Kentucky from data collected on core samples representing the complete section of the formation in three counties . Linear equations for estimating oil yield from measured specific gravity and for estimating specific gravity from measured oil yield were shown to be applicable within small error limits to all the sites tested . Variation in pyrite content is the largest source of error .

Jan 1, 1964

By M. H. Kersten, G. A. Brady, Jerry W. Ramsey

Anthracite samples were oxidized with nitric acid to prepare products representing intermediate stages of oxidation . Similar oxidizing conditions affected different anthracites to varying degrees as characterized by peptization behavior with 0.1 N NaOH . Techniques used in attempts to separate and characterize the products included esterification , absorption spectrophotometry , sublimation , chromatography , electrophoresis , metal salt formation , and solvent extraction . Mellitic acid , either free or in the form of metallic salts , was identified in the acid- soluble products from 10 tests in which the anthracite was treated with nitric acid for periods varying from 24 to 1,000 hours . pentacarboxylic acid was also found in some products . Other benzene carboxylic acids were not present in amounts detectable by the methods used in this study . The acid- insoluble residue from nitric acid treatment varied significantly in solubility behavior toward different classes of solvents . The most effective ones tried included polar oxygenated solvents and pyridine . Infrared spectra of the extracted material indicated that similar compounds were extracted by the different solvents . Aliphatic amines and aniline peptized the residue and o- toluidine reacted with it . Organic material separated from the residue by peptization with dimethylformamide contained 1 percent ash , consisting of more than 50 percent zirconium .

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 M. R. Geer

Three coals from the Wilkes on - Carbonado district of Pierce County , Washington , were subjected to washability analyses to estimate the amount and quality of washed coal obtainable . Because the coals were unusually difficult to clean , the washability examinations were supplemented by table tests , tests in dense - medium cleaning units , and flotation tests . None of the coals could be reduced to the desired 10 percent ash by tabling and the response to flotation by two of them was poor . Dense -medium treatment provided coal of the desired quality , but with the most difficult coal the recovery efficiency was lower than usual .

Jan 1, 1964

By T. F. Curry, L. B. Berger, H. A. Watson, S. J. Pearce

The conduct of work at elevated air pressures , such as in caissons and in tunnel - driving in subaqueous strata , poses safety problems not encountered in mining and tunneling operations at ordinary atmospheric pressure . This publication discusses some of the problems involved and presents information on the following subjects : ( 1 ) Physiological effects of gases at elevated pressure . ( 2 ) Use of respiratory protective equipment in rescue or recovery operations in event of fire or other emergency in pressurized tunnels . ( 3 ) Effect of elevated pressure on performance of some gasdetecting instruments ; interpretation of the results . Various types of respiratory protective devices are discussed in relation to their possible use at elevated pressures , especially the 2 - hour , selfcontained , recirculating - oxygen - breathing apparatus , which has had wide use in the United States during rescue and recovery work in the mining industry . A modified procedure that eliminates the hazard of oxygen poisoning enabling the safe use of this apparatus at elevated pressures , up to 45 pounds per square inch , gage , and tests to verify its practicability are described . procedure involves control of the partial pressure of oxygen in the breathing

Jan 1, 1964

By Harold M. Smith

The data in this report were prepared to show how Bureau of Mines routine crude oil analyses could be used to evaluate crude oils in terms of common commercial products . The use of Bureau of Mines routine analyses to determine hydrocarbon - type relationships for the gasoline and gas - oil fractions is demonstrated . For this purpose the correlation index , the aromatic profile and the naphthene profile are used to establish reasonably acceptable values for hydrocarbontype relationships . The derivation and meaning of these indications are discussed . These analytical interpretations are applied to a group of high - sulfur crude oils from the Near East , the Permian basin of West Texas , Venezuela , Colombia , California , and other locations , and the resultant data for gasoline , gas oils , lubricating oils , and asphalt are compared by appropriate tables and graphs . Because the Near East crude oils contain higher quantities of paraffins in the gasoline and gas oil ranges , they will yield good , lowsolvency solvents and good kerosine , jet fuel , and diesel fuels , but straightrun gasoline of inferior quality compared to similar products from either West Texas or Venezuelan high - sulfur oils . The Near East oils also should be good sources of lubricating stock . However , when used as stock for catalytic cracking or reforming , the Near East oils suffer by comparison because they are deficient in naphthenes .

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 D. E. Emerson, C. G. Kirkland, E. M. Frost

An apparatus has been developed for determining the helium content of gases containing 40 percent or more helium . It utilizes activated coconut charcoal at liquid nitrogen temperatures to adsorb constituents other than helium in the mixture . Series of analyses have been run where the mean deviation was less than 0.05 percent helium . Twenty or more analyses can be made in an 8- hour day .

Jan 1, 1964

By D. C. Crowell, A. G. Loomis

Both Dimensional and Inspectional Analysis are developed from fundamental concepts , and dimensionless groups are derived which represent the viscous , capillary , and gravitational forces existing in two - phase , incompressible flow in petroleum reservoirs . It is shown how properly scaled models may be devised by means of the foregoing groups . Laboratory measurements with such models faithfully duplicate the behavior of the reservoir on a miniature dimensional and compressed time scale , and when all the pertinent variables are evaluated , the model is a most effective tool for the study of complex fluid displacements in the reservoir . Applying the Principle of Similitude , it is shown how dimensionally scaled models are applied to various types of reservoir displacements : ( 1 ) Oil displaced by water , ( 2 ) gas displaced by water , and ( 3 ) miscible displacement . The special case of water displacing gas by imbibition is analyzed , and it is shown that the dimensionally scaled model must be fabricated of sandstone rather than unconsolidated sand , which is generally used in such models . This report is intended to be a review and summary of the application of Dimensional Analysis to reservoir displacement problems for those who are beginning the study of this useful and interesting method .

Jan 1, 1964

By W. D. Ludemann, E. A. Loria, E. A. Rowe

The isothermal recrystallization of electrorefined vanadium has been studied as a function of annealing time , temperature , and prior deformation . Specimens were cold- rolled from 30- to 75 - percent reduction in thickness , then annealed from 700 ° to 1,200 ° C at time periods ranging from 1 minute to 96 hours . The course of recrystallization was followed by means of hardness , metallographic , and X- ray techniques , and a recrystallization diagram was constructed . Interpretation of the data indicated that there was around 50- percent softening due to recovery ( first stage of softening) before recrystallization began . The defining of recrystallization limits with respect to the amount of deformation was precisely established for electrorefined vanadium . More than 30- percent reduction was necessary for recrystallization to occur at 850 ° C. With 60- percent reduction , it was initiated at 750 ° C and completed at 950° C. The activation energy for recrystallization , as derived from the data , was 95,300 cal per mole for 60 - percent reduction and annealing at 750 ° to 900 ° C. Recrystallization by the mechanism of nucleation and growth was the principal process during the second stage of softening . minor part of the second stage of softening took place as strain- induced boundary migration , which was observed in specimens reduced 30 percent , bent in L- shape , and annealed at 950 ° C. Grain size decreased significantly only with the largest reductions and annealing between 750 ° and 950 ° C. Grain growth was expressed by the empirical relation D = KKtt"" ,, the exponent being the same at 60- percent reduction and annealing from 750 ° to 900 ° C. Accordingly , the activation energy for grain growth was 75,000 cal per mole .

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

By M. E. Tyrrell, C. W. Houck

Mixtures of zirconium diboride and refractory metals of group VI were resistance sintered to high - density compacts using modified electric welding equipment . To evaluate the use of chromium , molybdenum , or tungsten as binders for zirconium diboride the sintered compacts were examined in polished sections and tested for crushing strength , hardness , microhardness , oxidation rate , and resistance to mechanical shock . Chromium yielded the highest compressive strength , the greatest resistance to mechanical shock and oxidation , and a satisfactory Rockwell hardness . Molybdenum did not yield a satisfactory cermet . Tungsten yielded compacts having high microhardness but very low mechanical strength .

Jan 1, 1964

By Robert M. Becker

This report (the second in a series of five) presents the mathematical development in extending 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 probability distribution functions (those here called the compound binomial and compound multinomial 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, while finite population moments are developed from corresponding infinite population moments using the finite probability operator defined in part 1 of this series.

Jan 1, 1964

By A. G. Starliper, H. Kenworthy

A procedure was developed for the separation of lead and sulfur in industrial concentrates of galena by a combination of chlorination and fused - salt electrolysis . Galena could not be satisfactorily electrolyzed in the various media tried ; however , when it was treated with chlorine the resulting lead chloride could be effectively separated electrically into lead and chlorine . An apparatus was designed and constructed to chlorinate galena and to volatilize simultaneously most of the chloridized impurities . By electrolyzing the chlorinated concentrate , a high percentage of lead was recovered . Anodic chlorine was drawn from the cell and was used to chlorinate new feed . In many runs , the recovered metal analyzed from 99.8 to 99.9 percent lead . Lead was also distributed as a chloride in the bath , and a small portion was in the volatile fraction produced during the chlorination step . During a tinuous operation , only 0.1 percent of the total lead was discarded ; 99.9 percent was accounted for in the metal , electrolytic bath , and washed or leached chlorination condensate which was essentially lead chloride . About 95 percent of the sulfur from the galena was recovered as a byproduct of over 90 - percent grade .

Jan 1, 1964

By K. K. Kelley, L. B. Pankratz

The heat contents of four silicate minerals -- akermanite , cordierite , gehlenite , and merwinite --were measured from 298 ° to around 1,700 ° K by the dropping method . The results were compiled into tabular and equation forms suitable for thermodynamic calculations . The heat contents of these compounds are nearly additive with respect to their constituent oxides .

Jan 1, 1964

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

The heat capacities of four crystalline silicates of barium ( BaSiO3 , BaSiO4 , Ba Si¸0 , and BaSi₂0 ) and two crystalline silicates of strontium (SrSio and Sr₂Sio ) were measured over the temperature range from 51 ° to 298° K. The results were used to evaluate the entropies at 298.15 ° K. The entropy values were joined with known heats of formation to obtain the free energies of formation of the silicates with respect to their constituent oxides at 298.15 ° K.

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 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 R. W. Hiteshue, R. W. Fridy, W. Kawa

A study of the production of coronene , a high - melting ( 440 ° C ) , highboiling ( 525 ° C) , polynuclear hydrocarbon , was made by the Bureau of Mines to determine the maximum yield obtainable by the hydrogenation of coal and coalderived materials . Experiments were made with anthracite and bituminous coals and with asphaltenes and centrifuged residue obtained from heavy oil produced in a pilot plant by the hydrogenation of a bituminous coal at 2,000 psi and 480 ° C. With anthracite , yields of coronene of 0.5 to 0.7 wt pct of moistureand ash - free coal were obtained at 6,000 to 8,000 psi , 700 ° to 750 ° C , and a residence time of 30 minutes . With bituminous coal , yields averaging 0.4 wt pct of maf coal were obtained at 6,000 psi , 800 ° C , and 30 minutes ' residence time . With asphaltene and centrifuged residue , yields of less than 0.02 wt pct of maf coal were obtained at 6,000 psi , 700 ° C , and 60 minutes ' residence time .

Jan 1, 1964