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By Rolland L. Blake

Petrographic and mineralogical studies were made on unoxidized samples from the Cuyuna and Mesabi districts to study occurrence and properties of the iron phyllosilicate minerals . Examination of 96 thin sections from the thinbedded facies of the main iron - formation of the Cuyuna district indicates that the most abundant minerals are Mn - Mg - siderite , stilpnome lane , and minnesotaite . Reconstitution and recrystallization of minerals has occurred along certain beds , and textures indicate that some minnesotaite apparently formed at expense of stilpnomelane . Three samples of stilpnome lane and one of minnesotaite were concentrated from fracture - fillings within iron- formation . Results of chemical , optical , spectrographic , X- ray diffraction , and differential thermal analyses on these samples are reported . The detection of ammonia in stilpnome lane samples is the first such occurrence reported , and its significance is discussed . New mineral data are presented on greenalite and probable septechamosite from the Mesabi district .

Jan 1, 1964

By D. W. Frommer, L. Bonicatto, M. M. Fine

A mineral - dressing investigation was conducted to demonstrate the ability of an anionic silica - flotation process to produce high- grade concentrates from submarginal iron ores of the western Mesabi and Menominee ranges . Commercially available equipment and reagents were used . Samples from the Menominee range were exclusively from the Groveland , Mich . , mine and contained hematite as the chief iron - bearing mineral . Bench- scale investigations established that the anionic silica flotation method can function effectively on a variety of undeslimed ores . Continuous tests completed on one Mesabi semitaconite ore and on Groveland mill feed , have verified the validity of the bench research . The Mesabi samples yielded a concentrate containing 60.3 percent Fe and 6.0 percent Sio with an accompanying iron unit recovery at 90.5 percent . Iron recoveries from the mill feed ranged from 79.0 to 87.4 percent .

Jan 1, 1964

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

Oil- yield data are presented for 40 sets of core samples and 83 sets of drill cuttings collected in 1952-62 from drilling operations in the Uinta basin of eastern Utah . This accumulated information on the location , extent , and richness of oil shales of the Green River formation is used to appraise the deposits as a source of oil and related products . Core samples used in the study were obtained specifically for evaluating oil shale , and they were satisfactory for this purpose , except they did not completely penetrate the formation . The drill- cutting samples were inferior to the core samples and yielded more erratic results . Consequently, oil yields based on cuttings should be regarded as indicative , rather than definite , until substantiated by other means . In general , the oil- yield data indicate Green River oil shale in Uinta basin is not as thick or as uniform as that in the Piceance Creek basin of western Colorado . However , it is an important potential source of oil . Estimates that beds 15 feet or more thick that average 25 gallons of oil per ton represent at least 120 billion barrels of oil in place are supported by the recent oil- yield data .

Jan 1, 1964

By Oliver Q. Leone

Three electrorefining cells were designed to investigate various factors associated with the electrorefining of reject - grade titanium sponge . Operation of the cells provided information on cell design as well as on how design and operating variables affected the quality of the titanium product . A sodium chloride - titanium chloride electrolyte was used , and the electrolyte chambers had capacities ranging from 400 to 3,500 pounds of molten salt . Major factors investigated were electrolyte composition , temperature and useful life , effect of various cathode shapes and materials of construction , methods for removing cathode deposits , effect of current density and cell potential , and the mechanics of deposit growth and crystal morphology . One of the cells was in intermittent operation over a 4 - year period and produced 2 tons of refined titanium . A product with a hardness of 80 or less Bhn (Brinell hardness number ) was consistently and easily obtained . Some metal with a hardness of less than 60 Bhn was produced . In one of the cells in which the electrolyte was held at operating temperature with an internal heater an ac input of 25 kw maintained 3,500 pounds of electrolyte at 850 ° C , but with an external heater 35 kw was required to maintain 400 pounds at 850° C.

Jan 1, 1964

By B. H. Eccleston, R. F. Kendall, D. E. Hirsch, Norman G. Foster

The mass spectra of 23 alkylthiophenes are presented , including 21 that have not been previously reported . Correlations between mass spectra and the structure of the thiophene homologs are discussed . Comparisons with , and corroboration of , earlier workers ' correlations and predictions are made . Several additional correlations are reported to enable the spectroscopist to identify the substituents on alkyl - substituted thiophenes , and the relationship of the mono - substituted and 2,5 - disubstituted alkylthiophenes is discussed in detail .

Jan 1, 1964

By E. G. Davis, H. P. LeVan, L. S. Smith

Leaching of a Georgia umber ore when using both ferrous sulfate and pickle liquor was studied in the laboratory . The ferrous sulfate content of the leach solution was the major factor affecting the extraction of manganese from the ore . Time , temperature , and the sulfuric acid content of the leach solutions had relatively little effect on leaching of manganese from the ore ; however , these factors did affect the amount of iron extracted from the umber and/or precipitated from solution . Simulated countercurrent leaching of the ore with pickle liquor containing 130 gpl (grams per liter ) ferrous sulfate ( 48 gpl ferrous iron ) produced a pregnant solution having 16 gpl manganese and 41 gpl iron . Filtration tests of the leach slurries indicated that separating the leach solution and solids by vacuum filtration was impractical , whereas pressure filtration was feasible when the cake thickness was limited to about three- fourths of an inch . Fired pellets of the filter cake yielded a firm , hard product analyzing 56 percent iron and less than 0.1 percent sulfur .

Jan 1, 1964

By A. Gene Collins, Cynthia A. Pearson, Cathy J. Waters

The chemistry of selenium and tellurium is discussed , along with a method of preparing a synthetic oilfield brine , an oilfield brine sampling method , and methods for determining selenium and tellurium in complex oilfield brines . Selenium either can be reduced to the elemental form with sulfur dioxide and determined semiquantitatively by color comparison of the red amorphous form or can be converted to selenite and determined quantitatively by reacting it with 3,3 ' - diaminobenzidine and obtaining its spectral absorbance at 420 mu . Tellurium can be reduced to the elemental form with hypophosphorous acid , and the spectral absorbance of its red hydrosol can be measured at 400 mu . Less than 0.05 mg / 1 of selenium and 0.1 mg / 1 of tellurium can be determined by the described methods .

Jan 1, 1964

By W. H. Frederic, F. H. Gibson, R. F. Abernethy

This publication contains the quantitative values for phosphorus , chlorine , sodium , and potassium in United States coals . The samples tested were taken from commercial shipments and have been selected to represent the principal coal producing areas of the country . Due to combining the analytical results from two separate surveys , values for the four elements are not available for all samples .

Jan 1, 1965

By Jr. Frank Parrish

This report describes the performance of 17 selected water-injection projects producing from Pennsylvanian-and Permian-age reservoirs. Illustrations depict reservoir structure and thickness, and production and injection history. A selected bibliography of publications pertaining to area oil recovery and geology is included. Tabulations of field and reservoir data reveal marked differences in the projects. Increased oil recovery resulted from injecting water in most cases; however, seven projects recovered less oil than the operators anticipated. Oil recovery by water injection ranged from 0.2 to 262 bbl per acre ft, or 0.1 to 22.5 pct of the initial stock-tank oil in place. Major reasons suggested for poor performance include: (1) Adverse directional horizontal permeability, (2) channeling of injected water through fractures or zones of high permeability, and (3) lack of containment of injected water. One 330-foot-deep project is among the first successful shallow water-floods in north Texas. Another project is the first successful Canyon sand-stone waterflood reported in the area. Previous gas injection in two Cisco sandstone projects did not prevent the reservoirs from responding favorably to waterflooding.

Jan 1, 1965

By Stephan Stecura

Crystallographic modifications and kinetics of solid-state phase trans-formations were determined for five rare-earth" sesquioxides--La2O3, Nd2O3, Sm2O3, Eu2O3, and Gd2O3. Oxides used for crystal modification studies were prepared by thermal decomposition of the following high-purity salts of the five rare-earth elements--carbonates, chlorides, fluorides, nitrates, oxalates, and sulfates. X-ray diffraction patterns of the cubic and hexagonal oxides were indexed by a graphical method and patterns of the monoclinic oxides by Ito's method. The kinetics of crystallographic transformation were determined by high-temperature X-ray diffractometry. The kinetic data were interpreted using a shrinking sphere model. All of the transformations followed first order kinetics. Activation energies were calculated by application of the Arrhenius equation. These solid-state phase inversions were concluded to occur by a reconstructive transformation mechanism.

Jan 1, 1965

By L. H. Adami

The heats of formation of anhydrous cadmium sulfate, cobalt sulfate, copper sulfate, nickel sulfate, and zinc sulfate were determined by hydrochloric acid solution calorimetry. The values at 298.15° K for formation from the metal, rhombic sulfur, and oxygen gas follow (cal/mole): CdS04J -222.0 ± 0.3; CoS04, -212.0 ± 0.4; CuS04) -183.4 ± 0.6; NiS04, -208.1 ± 0.2; and ZnS04, -233.1 ± 0.2. Corresponding heats of decomposition to form the metal oxide, sulfur dioxide, and oxygen were derived from these results; heats of decomposition to form the metal oxide and sulfur trioxide were also derived.

Jan 1, 1965

By T. C. Davis

Nine organic derivatives of fluorine, silicon, boron, and aluminum were purified for thermodynamic studies using distillation, zone melting, and gas liquid chromatography, The unusual properties of these compounds required the development of special techniques for handling and purification. To determine purities of purified samples, new techniques for analyzing spectral data were developed.

Jan 1, 1965

By Norman G. Foster

The mass spectra of 14 previously unreported alkylthiophenes are pre-sented. Low ionization voltage data of selected compounds from these 14 and 23 previously reported alkylthiophenes are presented and discussed for their value in supporting fragmentation mechanisms analytical correlations. A comparison with and corroboration of earlier correlations is made. Additional correlations concerning detection of side chain branching and the detection of ethyl-alkyl and propyl-alkylthiophenes are made. A discussion of the possible fragmentation routes and mechanism of fragmentation is given. Speculative structures are inferred s out some of the ions and hence this work provides a basis for suggesting fation mechanisms for the alkylthiophenes according to modern theories ass spectrometry. Verification of these mechanisms must await the availability of isotopically labeled molecules which are labeled in specific lotions that permit the definition of the paths of frag-mentation. Some suggestions for further work to generalize on the correlations and studies made to this point are presented.

Jan 1, 1965

By Jr. Smith

The equilibrium compositions of product gases for mixtures of air with methane, propane, or ethylene at and around flame temperatures are reported. For each hydrocarbon, compositions are given for five fuel-to-air ratios--two lean, two rich, and one stoichiometric--at five pressures, from 1 to 20 atmospheres, and at an ambient temperature of 25° C.

Jan 1, 1965

By Glenn L. Cook

Correlations between mass spectra and molecular structures of 186 organic sulfur compounds are discussed. The olefinic ions, the alkyl ions, the CnE2n+1 ions, the m/e 61 ions, and the m/e 35 ions in the spectra of thiols are related to molecular structure. In the spectra of sulfides, the olefinic ions, the m/e 61 ions, the m/e 35 ions, the CnH2n+1S+ ions, and the CnH2n+1SH+ ions are correlated with molecular structure. For disu1fides, the correlations relate HSSF+& and RSSH+ ions to molecular structure. Base peaks of alkylthiophenes are correlated to their molecular structures. Some unimolecular reactions of sulfur compounds in the mass spectrometer are considered. A cyclic intermediate is suggested for the reaction which produces m/e 47, CH3S+, and m/e 48, CH4S+, ions in the spectra of sulfides. An expanded ring is suggested as a possible intermediate in the reactions of thiophenes. Heats of formation of sulfur-containing ions and their appearance potentials are presented in tabular form. Ionization potentials for sulfur-containing radicals and molecules are also given. Discussion of the spectra, tabulated in the appendixes, provides an insight into the relationship of the molecular structure of a compound to the mass-to-charge ratios and the intensities of the ions in its mass spectrum. Correlations of the mass spectra with molecular structures are empirically developed by observing regularities in the spectra of the reference compounds. Correlations extend the usefulness of mass spectra because they can be employed to determine the molecular structure of an unknown compound.

Jan 1, 1965

By Lippe D. Sadwin

This report describes a high-speed streak camera technique for measuring the lateral shock pressure generated by a cylindrical explosive charge detonated from one end. Experimental data show that the magnitude of the lateral pressure is approximately 50 percent that of the pressure generated from the terminal end of the charge for three explosives studied.

Jan 1, 1965

By Raymond L. Lowrie

Coal deposits in the Boulder-Weld County coalfield in Colorado are analyzed in relation to economic factors governing the growth, stability, and competitive potential of the coal industry. Recoverable reserves, estimated to be 571 million tons, are discussed in detail, particularly those in the Erie and Frederick Quadrangles. Geology of the coal measures, quantity and quality of water resources, and chemical and physical properties of the coal are described. Coal production factors, including mining techniques and equipment, labor requirements, transportation facilities and rates, and markets, are considered for coal's position in competition with alternate fuels. Growth of the fuels market, through increasing thermal-electric power generation in the Denver Metropolitan Area, will stimulate coal production in Colorado. Reserves of the contiguous Boulder-Weld coalfield, if mined in a sustained, year-round, high-tonnage operation, could be used to supply much of that fuel demand.

Jan 1, 1966

By John J. Mulligan

The Bureau of Mines investigated the tin deposits of the Cape Mountain area during July and August 1962 to test the effectiveness of detrital-cover sampling in permafrost areas as a relatively cheap and simple means of guiding mine development and exploration. Results indicate that systematic detrita1-cover sampling can be used effectively to delineate obscure deposits with sufficient accuracy to permit sampling with a minimum of trenching or drilling. Extensions of known outcroppings were traced in sufficient detail to guide lode sampling and several previously unknown tin-bearing lodes were found and sampled. Lode sampling was limited to the minimum needed to establish the reliability of detrital-cover sampling results. The results of previous lode and placer investigations are summarized and detrital-cover sampling methods and results are described in detail.

Jan 1, 1966

By Norman G. Foster

The mass spectra of four tertiary butyl substituted thiophenes are reported. A comparison and contrast with earlier structure correlations made by API-RP48 mass spectroscopists is presented. The fragmentation routes of these types of molecules are discussed and explained in terms of existing theories in mass spectrometry. Low ionization voltage data are presented to support the mechanistic picture developed. Structures are inferred about some of the ions, and these are correlated with existing theories. Metastable peaks in the spectra are used to support the fragmentation paths. The presence of doubly charged ions in the spectra is noted and the possible implications toward mechanisms discussed. The general picture of simple, small fragments leaving the ion moiety upon further fragmentation is developed in detail. Some suggestions are presented for further work utilizing isotopically labeled molecules to establish firmly the general picture of fragmentations of the alkylthiophenes.

Jan 1, 1966

By Alton B. Cook

A material balance equation was derived for calculating (1) the initial oil volume and (2) the relationship of average reservoir pressure to net gas in storage in reservoirs used for natural gas storage operations. The equation is also applicable to secondary-recovery operations where reservoirs are completely repressured and gas cycled. Using this equation minimized two probable sources of appreciable error in conventional material balance calculations: inaccurate measuring of and accounting for produced gas, and differences between true reservoir pressure and average reservoir pressures as derived from bottom-hole pressure measurements. A new procedure is presented for calculating water encroachment. By solving the conventional material balance equation and the derived equation for gas storage simultaneously, the values for initial oil in place and net water encroachment can both be determined.

Jan 1, 1966