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By J. G. Donaldson

A bench-scale method for recovering lead and zinc from slimes and mill tailings from the Tri-State District of Missouri, Oklahoma, and Kansas was developed by the Bureau of Mines. Dilute hydrochloric acid, containing sodium chloride, and chlorine gas were used to decompose the mineral constituents. Lead was electrolyzed from the pregnant acid solution, and zinc was precipitated from the depleted electrolyte by neutralization with lime. Up to 98 percent of the lead was recovered in an impure lead electro- deposit assaying approximately 85 percent lead. Zinc recoveries up to 90 percent of the total were attained in a precipitate assaying approximately 40 percent zinc.

Jan 1, 1963

By C. O. Hawk

As an exploratory effort to produce useful products from coal by a new path, the Bureau has made a few experiments on the fast heating of finely ground coal particles by irradiation with a flash of high intensity light. The flash was produced by an electrical discharge at high voltage through a xenon-filled tube. The flashes lasted from 2 to 3 milliseconds. The reaction took place in small sample tubes, ½ inch-dimeter by 4 inches long, and with small amounts of coal (total amount charged 0.1 gram, probable effective amount not more than 20 milligrams). Average particle size of the coal, estimated on a numerical basis, was 20 microns. Temperatures reached were evidently quite high, because all products obtained in quantity were characteristic of high temperature pyrolysis. Apparently, conversion of the coal was extensive where isolated particles received the full benefit of a flash. It seems particularly significant that acetylene was present in appreciable amounts--comprising almost 3 percent of the total gaseous product in one case. This is good evidence of a short heating period to very high temperature (well above 1,000° C) followed by rapid quenching. Although the results are interesting, they do not suggest any immediate practical application.

Jan 1, 1963

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 C. M. McKinney

This report contains Bureau of Mines analyses of 291 samples of crude petroleum from the Gulf Coast Area of Louisiana and Texas. Included are 65 analyses from 51 Louisiana fields and 226 analyses from 216 Texas fields. Analyses from the Texas fields include 90 from 58 Upper Gulf Coast fields, 47 from 28 Middle Gulf Coast fields, and 89 from 40 Lower Gulf Coast fields. The analyses represent fields that produced 1,000 barrels or more per day during at least one of the years 19.57 through 1961, with the exception of 23 analyses from the Texas fields. The fields considered are listed by state and geographical groupings, with field names arranged alphabetically within each grouping. The tabulation also includes information concerning the geological sources of the samples. General characteristics of the crude oils and analytical and computed data determined from the analyses are summarized. Crude oil production data are given for the fields for 1960 and 1961 and are cumulative through 1961.

Jan 1, 1963

By Earle S. Burnett

This report outlines the experimental procedures for using a Burnett apparatus to obtain compressibility coefficients for multiphase, multicomponent fluid mixtures. The conventional Burnett method is described briefly whereby multiphase compressibility data can be obtained by first determining the compressibility factor, Z, as an isothermal function of pressure alone. Then starting at conditions of temperature and pressure where Z is known, the fluid is cooled at constant volume to some lower temperature at which the resulting pressure is measured, and a corresponding value of Z is obtained from a fundamental relationship between compressibility factors, pressures, and temperatures at constant volume. The isochoric treatment of the fluid, extended to still lower temperatures and along other isochors, eventually results in compressibility determinations for the whole two-phase system thus covered experimentally.

Jan 1, 1963

By Thomas L. McVay

Laboratory batch and pilot plant flotation tests were made to determine the feasibility of recovering commercial grade kyanite from a quartzite- kyanite rock from the Graves Mountain, Ga., deposit. Best results in laboratory and continuous tests were obtained using sodium carbonate for pH control, citric acid for quartz depression, and oleic acid as the kyanite collector. Over 80 percent of the kyanite was recovered in a concentrate analyzing 56.8 percent Al203 and 3.8 percent hydrochloric acid soluble Fe203. Subsequent treatment of the flotation concentrate by magnetic separation reduced the acid soluble Fe2O3 to 0.6 percent and increased the alumina content to 59.2 percent. Acid leaching of the concentrate gave a product analyzing 59.7 percent Al203 and about 0.1 percent Fe203. As a result of the beneficiation research, a commercial kyanite flotation plant was completed in September 1962 by private industry.

Jan 1, 1963

By A. F. Baker

Tests were conducted in commercial foundries to determine the suitability of calcined anthracite as a cupola fuel. The calcined anthracite performed satisfactorily at two of the three foundries where iron-melting tests were conducted. Performance at the third installation was unsatisfactory because metal temperatures deviated widely and, in general, were lower than is desirable for the type of castings being made.

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 Earl L. Hastings

Although the principal market for diatomite in the United States is in the East,4 production of the material is presently restricted to the West, because the deposits are larger, mining costs are cheaper, and the quality of product is better than that obtained from other domestic deposits. However, Tallahatta diatomite, occurring in Choctaw and Clarke Counties, Ala., has a freight rate advantage, which should encourage competition for those market that are now being supplied with the purer diatomites from the western deposits. For this reason, diatomite occurrences in the Tallahatta formation were examined by the Bureau of Mines and physical properties of samples from the deposit were determined to obtain additional data for use by any potential producer who wished to evaluate the material for its commercial possibilities. In 1894 K. M. Cunningham5 found that the buhrstone formation (now known as the Tallahatta formation) contained "siliceous shells of marine diatoms, radiolaria and foraminifera, thus being rather of the nature of tripoli or diatomaceous earth than of a true clay." Cooke6 and Semmes7 also reported the Tallahatta formation to be composed principally of diatomaceous earth with accompanying beds of sand, clay, and sandstone.

Jan 1, 1963

By Michael Sokaski

A dense-medium cyclone pilot plant was built to clean 112-inch to 0 size coal. This pilot plant does not require the removal of the extremely fine material (usually minus 1/2-mm) from the feed, which is necessary in conventional dense-medium cyclone plants. The essential difference between conventional cyclone plants and the pilot plant is in the medium-recovery system. The latter uses a combination of sieve bend screens, classifying cones, and magnetic separators for medium recovery. Eight tests were run in the pilot plant at a feed rate of 5 tons per hour with four different raw coals and one crushed jig middling product. Sharp separations were obtained as indicated by an average error area of 27 and probable error of 0.047 for the 112-inch to 200-mesh size range. Magnetite loss averaged about 2.5 pounds per ton of feed. The influence of several factors on cleaning performance of the cyclone was investigated. The diameters of both the overflow and underflow orifices were found to be important for optimum cleaning performance, but these diameters could vary over a wide range without serious effect; however, if this range was exceeded, cleaning performance deteriorated. Better cleaning performance was obtained when the cyclone inlet pressure was increased from 9 psig to 13 psig. The size of the magnetite particles in the medium was found to have a substantial effect, and the best cleaning results were obtained with grade B magnetite. Demagnetizing the magnetite in an effort to decrease the effective particle size did not improve cyclone performance.

Jan 1, 1963

By H. E. Powell

This study was made to determine the capabilities and limitations of the hydrocyclone for separating quartz sand from impure clays, Optimum operating conditions for beneficiating typical subgrade clays were determined. Estimates are furnished for installation and direct operating costs of hydrocyclones in such separations. Laboratory models of commercial hydrocyclones were used to beneficiate a suite of fire clays including plastic, semiflint, and flint types, all of which were contaminated with quartz in amounts ranging from 3 to more than 62 percent. Results show that this technique is not limited to a single type of clay but is applicable to clays ranging from plastic through flint, Under proper conditions use of this technique will result in good separation of the sand and good recovery of a useful clay mineral concentrate. Rejection of quartz from the clays investigated ranged from a low of 82.4 percent with an alumina recovery of 71.2 percent to a high of 99.0 percent with an alumina recovery of 85.6 percent.

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 Lowell Stroud

A windowed-cell phase equilibrium apparatus was used to obtain equilibrium vapor- liquid data for a helium-bearing natural gas (Hogback) at temperatures from -100 to -250° F and pressures to 500 psia. Anomalous phase behavior resulting in the formation of two stable liquid phases occurred at tmperatures below -200° F and pressures above 200 psia. A review of the published literature on the occurrence of multiple-liquid phases included in the report indicates that the experimental results with Hogback gas are the first substantiated evidence of a vapor-liquid-liquid equilibria in a helium-containing natural gas.

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 NIOSH NIOSH

This work explores application of a double alkaline leach method to extraction of alumina from Oregon ferruginous bauxitic materials. The process recovers a greater proportion of alumina from high-silica ores than is possible by a conventional single-leach method. This recovery is accomplished by calcining the ore, removing reactive silica in a preliminary dilute caustic soda leach, and then applying a second leach to dissolve alumina. Ores containing up to 15 percent Si~) 35 percent AI;:) Os, and 30 percent Os were examined. Under conditions of treatment established by experimentation, more than BO-percent alumina extraction was demonstrated. When and if conditions demand the use of low-grade materials, the double-leach process is capable of providing millions of tons of alumina from Oregon ferruginous bauxite.

Jan 1, 1963

By J. M. Seward, W. D. Dietzman, M. E. Hawkins

Analytical studies of formation waters are widely used by the petroleum industry as an aid in solving problems such as identifying intrusive waters , corrosion studies , treating injection water , and choosing open or closed water- injection systems . The solution of a problem is often simplified when reliable analyses of the waters under consideration have been made previously . Chemical analyses and electrical resistivity measurements are presented on 267 samples from 74 fields in south Arkansas , and 199 samples from 80 fields in north Louisiana .

Jul 1, 1960

By W. R. K. Wu

Studies are reported on the structure of coal and coke with the graphical , statistical densimetric method based on the relation between the molecular volume per carbon atom ( M / C ) and the atomic hydrogen - carbon ratio ( H / C ) . Previous work , mostly from chemical and physical investigations , is critically reviewed . Difficulties in evaluating the ring increment are demonstrated for coal and coke for the statistical densimetric method based on the additivity of atomic volumes of constituent elements . A new diagram is presented for the graphical method . Methods are introduced for correcting M /C and H/C for the presence of minor constituents in coal and coke . With the graphical method , the fractions of aromatic carbon atoms in the total carbon atoms are estimated for a coal , a resin , and 5 petrographic components ; the types of condensed structure in the fundamental units of molecules are discussed for these substances , 28 coals , and 6 " average " cokes at 500 ° to 1,000 ° C. It is also shown that the number of rings in the fundamental units of coal generally increases with increasing rank and that of coke , with increasing carbonization temperature .

Jul 1, 1960

By C. J. Chindgren, L. C. Bauerle, J. B. Rosenbaum

Modifications of the conventional method of preparing ductile vanadium metal by calcium reduction of V2 05 in a bomb were explored for clues to a more economical procedure . The modifications examined included ( 1 ) omitting the gas purge of the bomb ordinarily used for eliminating atmospheric nitrogen , (2 ) using low- grade vanadium feed materials , ( 3 ) using alternative reductants , such as aluminum , magnesium , and silicon , and reductant mixtures , and ( 4 ) bomb refining of aluminothermic metal produced in open- vessel reductions . The most promising modification appeared to be bomb refining , using calcium to purify vanadium metal -- of low aluminum but high oxygen content-- prepared by open- vessel aluminothermic reduction of vanadium pentoxide .

Jul 1, 1960

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

Fluidized - bed roasting was investigated as a means of decomposing gypsum and gypsum mixtures to produce a gas rich in sulfur dioxide and a lime or portland cement residue . Ninety- eight percent desulfurization of gypsum in a 10 - inch fluidized- bed reactor took 1.5 hours at an operating temperature between 1,200 ° and 1,225 ° C. A cement- type residue was obtained but had to be refired at 1,450 ° C before mortar prepared from it met the physical specifications for cement .

Jan 1, 1963

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

Mullite is a substance of prime importance in ceramic technology . Despite this fact , its thermodynamic properties have received little attention . A Bureau of Mines literature survey disclosed the absence of lowtemperature heat capacity data , the absence of an experimental entropy value for 298.15 ° K , and the lack of heat content data beyond the temperature range from 298° to 576 ° K. Data supplied in this Bureau report fill these gaps in the thermodynamic knowledge of mullite . According to equilibrium phase studies of Aramaki and Roy ,3 the mullite phase melts congruently at 2,123 ± 15 ° K , and the equilibrium crystallinephase composition extends from Al Si2013 to Al6.8 Si₂ Q4.2 . The results in this report are for the stoichiometric composition , Al Si¿Qз . • Heat capacity measurements were made over the temperature range from 50 ° to 298 ° K , and the entropy at 298.15 ° K was evaluated . Heat content measurements covered the temperature range from 298 ° to 1,800 ° K. Heat content

Jan 1, 1963