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By O. Terichow

A pendulum sclerometer designed by the Bureau of Mines is described. Its method of operation is given, along with the results of tests made on representative mineral samples of Mohs' hardness scale to determine the applicability of the device for research on rock testing. The sclerometer hardness values obtained from the tests indicated that reproducibility and accuracy were good. A quantitative comparison of the pendulum hardness values with microhardness and surface energy values published by other investigators showed good agreement on minerals with Mohs' hardness numbers of 2 to 9.

Jan 1, 1967

By Jr. Hazen

Two statistical techniques, the mean-square-successive-difference test and correlation, are used to investigate the problem of assigning an area of influence to an assay. Data from five hydrothermal deposits, Climax molybdenum, Cebolla Creek titaniferous iron, San Manuel copper, Piedra Hueca copper, and Butte copper, are studied. Two groupings of the assays are used for the mean-square-successive-difference tests. One group involves an increasing sample volume by reaveraging assays to represent a longer sample intervals, the other by regrouping assays to represent longer sample intervals without a change in sample volume.

Jan 1, 1967

By J. M. Singer

Methods are proposed for predicting concentrations of nitrogen oxides and carbon monoxide in the combustion gases of flames, specifically of lean, stoichiometric, and rich propane-air flames. Calculations are based on kinetic and thermodynamic theory. These theoretical data are compared with concentrations observed experimentally downstream of flat grid-type burner flames (approximately 25,000 Btu/hr) that were used to simulate gas appliances such as water and space heaters. Air pollutant concentrations are also computed for (1) flames chemically perturbed by recycling flue gases into the primary fuel-air mixtures; (2) flames thermally perturbed by cooling the burned gases at different rates; and (3) flames perturbed by combination of these two effects. In general, experimental and computed concentrations agree to within a factor of 2 to 7 with the experimental values always being higher than the theoretical. The theoretical analysis indicates that cooling the primary flame by recycling cold flue gases (with and without excess air) reduces the relative emission of nitric oxide and increases emission of carbon monoxide if the flame stoichiometry does not radically change. Cooling rates of about 5,500° to 10,000° R/sec starting at about 3,500° R generally suffice to prevent nitric oxide concentrations in lean flames from increasing much above the initial values at the combustion zone; these same cooling rates do not prevent oxidation of most of the initial carbon monoxide.

Jan 1, 1967

By Jr. Fish

As a part of a study of iron are resources in the Appalachians, 9 diamond drill holes aggregating 1,580.7 feet were drilled in a portion of the Butt Mountain area of northeastern Giles County, Virginia. Three hematitic sand-stone beds were intersected in the Clinton formation but only one was consistent in thickness and grade in all 9 drill holes. This bed averages 18.9 percent iron over an average thickness of 24 feet. The drill cores were logged and chemical analyses were made on 161 individual samples and 22 composite samples. Beneficiation studies were made of three composite hematitic sandstone samples each representing a separate bed containing 14.6, 19.8 and 20.0 per-cent iron. Major mineral constituents of the samples were hematite, quartz, and sericite.

Jan 1, 1967

By Henry M. Harris

A study was made by the Bureau of Mines to determine if shapes of oxide-glass compositions could be roll-formed at high temperatures, and to find the conditions required for adequate formability. A unit with directly connect' furnaces and heated rolls that allowed forming of most of the compositions developed. Glasses of the feldspar type were chemically unreactive with the alumina grains, and allowed the best roll forming. Optimum forming was attained at temperatures of 1,400° to 1,530° C, with compositions containing 30 or 40 percent feldspar and 60 or 70 percent alumina. Formability was better when compositions contained minus 325-mesh materials, rather than coarser or finer powders. In many cases, roll-formed shapes had physical properties equal to or better than the normally sintered shapes of the same composition.

Jan 1, 1967

By Jack L. Henry

The monocarbide region of the ternary system U-C-O has been investigated at 1,700° C as the first phase of a more extensive study of a portion of the four-component system U-C-O-N. An area bounded by the following compositional limits in atomic percent was studied: U, 44 to 55; C, 30 to 60; 0, 0.2 to 20. Compacts composed of mixtures of uranium, graphite, and uranium dioxide powders were sintered at 1,700° C under an equilibrium pressure of carbon monoxide to produce uranium oxycarbide specimens having a variety of compositions. Sintered specimens were evaluated by X-ray, chemical analysis, and ceramographic techniques. Solid-solution boundaries and phase relations have been established, and the effects of composition on the lattice parameter as well as the decomposition pressure have been investigated. Oxygen can be substituted for carbon in stoichiometric uranium monocarbide to the extent of about 17 atomic percent at 1,700° C. The composition range of the oxycarbide solid solution extends from about 48 to 51 atomic percent uranium in the low oxygen region. Above 10 atomic percent oxygen the composition range narrows to less than 1 atomic percent uranium. Carbon monoxide exists as a gaseous phase in equilibrium with all compositions which contain oxygen. Five separate phase fields were found bounding the solid-solution area. Other phases within this portion of the system include uranium, uranium dioxide, uranium dicarbide, and uranium sesquicarbide. Decomposition pressures of oxycarbide compositions at 1,700° C have been found to vary from a few microns for stoichiometric and uranium-rich compositions to 35 torr for carbon-oxygen-rich specimens. Lattice parameters were found to depend upon the U to C + 0 ratio as well upon the extent of substitution of oxygen into the stoichiometric monocarbide lattice.

Jan 1, 1967

By R. B. Tippin

The heavy liquid separation (HLS) process was investigated by the Bureau of Mines to develop a means of concentrating minerals from natural ores, Various spodumene ores were tested in a 0.4-inch diameter cyclone using pure tetrabromoethane (TBE) as the heavy liquid. Studies were initiated to examine the influence of (1) pulp density (2) feed grade, (3) cyclone pressure, (4) cyclone apex opening size) (5) cyclone vortex finder opening sand (6) mineral particle size on the separation efficiency. Each of these factors was found to affect the heavy liquid separation in some degree; the mineral particle size exhibited the greatest effect and the ore feed grade the least. Conditions necessary to yield an 85 percent spodumene concentrate with an 85 percent recovery were determined to be: 70 psig pressure, 10 percent solids, 0.08-inch apex opening, 0.11-inch vortex finder opening and a minimum amount of minus 200-mesh fines in the feed. Operation of multiple cyclones in series resulted in spodumene concentrates assaying over 90 percent and indicated mineral recoveries exceed-in 90 percent.

Jan 1, 1967

By K. P. V. Lei

The Bureau of Mines investigated molten salt electrorefining 'n helium atmosphere cells as a means for the production of ductile vanadium. 'Electrolytes composed of NaCl-VCl2, LiCl-NaCl-VCl2, BaCl2-KCl-NaCl-VCl2 KCl-LiCl-VCl2, and CaCl2-NaCl-VCl2 were tested. Two electrolytes, KCl-LiCl-VCl2 and CaCl2-NaCl-VC12, were selected for laboratory-scale production tests. A molten salt electrorefining process was developed for the production of ductile 99.6 percent vanadium from a commercial 90-percent grade. Using the CaCl2-NaCl-VC12 electrolyte, an 87-percent recovery of ductile vanadium was made; an 85-percent recovery was made with the KCl-LiCl-VCl2 electrolyte.

Jan 1, 1967

By Hillary W. St. Clair

The reduction zone of the iron blast furnace is represented by a mathematical model of the chemical reactions and heat transfer that occurs between gas and solids during the deoxidation of iron oxide. The model consists of a set of equations and an algorithm whereby the equations may be solved to give the temperature and composition of gas and solids at any position in the reaction zone and at any time after a specified initial state. The model is applied to the special case in which ferric oxide is reduced by graphitic carbon and carbon monoxide produced by burning carbon in dry air. The rate of reduction, carbon consumption and maximum temperature are shown as functions of the temperature and rate of flow of the incoming reducing gas and external heat loss. The model of the reduction zone is the essential part of a general mathematical model for simulation of the iron blast furnace. The simulation model will serve as a research tool to be used in conjunction with an experimental or operating furnace. After the simulation model has been correlated with the real furnace, it is proposed that further experimentation be done mostly with the model. The real furnace will then be operated primarily to test and confirm the model.

Jan 1, 1967

By R. T. Sorensen

Bench-scale and continuous testing were performed to adapt the anionic process for flotation of calcium activated silica to the fine-grained hematitic-goethitic jaspers from the Marquette range, Michigan. These ores typically contain about 35 percent Fe and require grinding to about 80 to 100 percent minus 400 mesh to insure an adequate liberation of gangue from the iron oxides. A method for removal of troublesome slime fractions without excessive iron loss, by first dispersing the quartz and then selectively flocculating the iron oxides, was evolved in the laboratory and successfully accommodated to pilot plant practice. The efficiency of the flotation process was improved with respect to both reagent usage and concentrate grade and recovery by using the selective flocculation-desliming technique as a pretreatment. The benefits of the combined desliming-flotation procedure were most evident in pilot plant processing. The best tests on two ores yielded recoveries of about 84 percent in concentrates containing 65.1 percent Fe and 4.8 percent SiO2 and 66.2 percent Fe and 3.9 percent SiO2, respectively. These results are in comparison to recoveries about 10 percent lower than the above to concentrates containing 63.9 percent Fe and 6.6 percent SiO2 in the one instance, and 63.6 percent Fe and 7.2 percent SiO2 in the other, obtained by flotation without the prior desliming treatment.

Jan 1, 1967

By Maurice Deul

A special short-term research project was initiated to develop plant design parameters for treating mine waters to yield an effluent acceptable for discharge into streams and a sludge amenable to effective and economic disposal. Neutralization was investigated to provide simple and direct treatment of ferruginous acid waters using lime; coarse limestone, and limestone followed by lime. Limestone treatment was accomplished using a small cement mixer as a simple reactor to provide abrasive agitation of limestone and mine water. Results from tests with nine mine waters encompassing a wide range of iron and acid concentrations showed that coarse limestone, one of the cheapest neutralizing agents known, is potentially useful for treating mine water discharges. However, process variables must be defined more completely before the practical applications and limitations of the process can be fully established. In all the tests a pH of >7.2 was obtained ultimately with limestone. Reaction time to reduce the iron content below 7 ppm in the water was dependent on the original ferrous iron concentration. For waters with high ferrous iron content, treatment with limestone followed by lime rapidly produced an acceptable treated water, Sludges with good settling and handling characteristics resulted when limestone was used for neutralization either alone or with subsequent treatment. Reaction rates are expressed graphically as pH change and iron depletion curves; characteristic solids settling curves are shown. The temperature dependency of ferrous iron oxidation was verified.

Jan 1, 1967

By Renpei Yoda

An investigation was conducted to develop columbium alloys with e1evated-temperature strengths higher than those exhibited by more common commercial columbium alloys, and attention was given to improving the oxidation resistance and ease of fabrication. Additions of carbon, aluminum, and chromium were made to some columbium-base alloys, and their effects on workability, recrystallization, oxidation resistance, and mechanical properties at elevated temperatures were explored. The additions were made to take advantage of (1) solid solution strengthening, and (2) precipitation hardening. Three alloys displayed good high-temperature properties with relatively good oxidation resistance at 1,000° C, and tensile strengths from 26,000 to 32,200 psi at 1,400° C. When the properties of these alloys were compared with those of commercial alloys, B-66 and FS-85 (1),4 the outcome was favor-able for the alloys studied in this investigation.

Jan 1, 1967

By L. F. Heising

Ten composite samples of Mesabi Range nonmagnetic taconite from the Hibbing, Minn., area were evaluated by flotation and by reduction roasting-magnetic separation to determine their potential as a future source of iron are. Only one of the composites yielded concentrates that could be considered marketable, using as a criterion a 10-to-1 iron-to-silica ratio. Cursory petrographic examinations of all 10 composited samples and a detailed mineralogical study on 1 sample suggest that unfavorable mineralogical associations between iron and gangue minerals are responsible for their poor beneficiation characteristics.

Jan 1, 1967

By Karl-Heinz Frohne

This report presents the findings of a study of a portion of the Clover-Rush Run oilfield located in Roane County, W. Va. The study was made to investigate the possibilities of secondary oil recovery in the Big Injun sandstone underlying the William Kaufman lease. Reservoir properties, original reserves, and primary oil recovery are also presented. The investigation is based on a core analysis and related laboratory tests, well records, field production data, and subsurface information from the Kaufman property. A theoretical primary oil recovery of 9.7 percent of original oil in place is predicted for the reservoir. A waterflood performance prediction of a hypothetical pilot area was made by use of a computer. The prediction showed that, based on laboratory oil water relative permeability curves, the water-injection time needed to initiate oil production is excessive and that the stabilized water-injection and corresponding oil-production rates are very low. This precludes waterflooding the reservoir on an economic basis. A prediction for secondary oil recovery by gas injection was attempted but could not be completed because essential reservoir data were not available. In July 1965, the lease operator initiated, and is currently conducting, a gas-injection program, but there had been no increase in oil production up to November 1966.

Jan 1, 1967

By Glenn E. Johnson

The Bureau of Mines investigated the production of hydrogen cyanide by reacting powdered coal (minus 300 mesh) with ammonia at 1,250° C in a bench-scale study. Both metallic and ceramic reactors were used. Yields up to 0.7 cu ft of hydrogen cyanide per cubic foot of ammonia consumed r- obtained. The resulting ammonia conversion of about 75 volume-percent approximates conversion obtained commercially in processes utilizing natural gas and platinum catalysts. The coals that had higher volatile-matter contents gave the best yields of hydrogen cyanide. Allowing the coal to adsorb ammonia before reaction resulted in increased yields of hydrogen cyanide. Cost studies for a plant with a 40-million-pound-per-year capacity indi-cate that hydrogen cyanide can be profitably coproduced with carbon black, from coal and ammonia, at the current market price of hydrogen cyanide (11.5 cents/lb). These figures are based on heating the reactor electrically. If a cheaper heating method were devised the economics of the process would be more favorable.

Jan 1, 1967

By Robert W. Ageton

Optimal planning for mining the deep, lead-zinc-silver deposits of the Coeur d'Alene mining district, Shoshone County, Idaho, could be facilitated by a knowledge of the magnitude and direction of the pressure acting in the virgin rock. The distribution of primary stresses should be considered in order to prevent possibly destructive mining-induced stress concentrations. This particular investigation was concerned with determining stress in a zone 4,000 feet below the surface and known to be ender stress concentrations due to mining operations. Disking of the stress-relief cores obtained in a vertical down hole permitted qualitative evaluation from visual observations; the results indicate that a high lateral stress existed at the time the measurements were made. Stress-ellipsoid determinations gave a compressive principal stress of -13,000 psi oriented about N 45° W and nearly horizontal, a compressive principal stress of -11,000 psi oriented about S 45° W and abut 60° off the vertical pointing away from the vein, and a compressive principal stress -5 -7,000 psi oriented N 45° E and about 60° off the vertical, pointing toward the vein. Subsequent to the overcoring stress-relief drilling, a rock burst occurred about 100 feet northwest of the test site.

Jan 1, 1967

By Wilson Blake

The Bureau of Mines used a mathematical model based on the finite element method of stress analysis to calculate stresses and displacements surrounding an open pit mine in a gravity-loaded rock mass. Comparison of the finite element solution for a semicircular notch in a gravity-loaded plate with the theoretical solution for a semicircular notch in a plate under uniform compression parallel to the free boundary demonstrates the inapplicability of the latter method to openings at the free surface of a gravity-loaded medium. High stress concentrations are formed at irregularities along the boundary of an open pit in a gravity-loaded continuous competent rock; however, for this type of rock the magnitudes of the stresses are too low to be considered a major factor in open pit slope stability. High stress magnitudes will occur if, in addition to the gravity stress field, a large horizontal stress field exists.

Jan 1, 1967

By R. V. Higgins

The Bureau of Mines investigated the use of electronic computers for obtaining more information about relative permeabilities of reservoir rock to oil and water. It was found that there are many possible combinations of relative permeability curves that will result in virtually the same recovery versus injection) but they require different times and rates to recover the oil even with different mobility ratios. Permeability curves obtained by the use of non-viscous oil and employed for calculating the waterfloods of viscous oils can lead to serious inaccuracies. For viscous oils) the wettability characteristics in the middle portion of the permeability curve affect recovery nearly as much as other portions of the curve; this) however) is not true for non-viscous oils in water-wet reservoir rock.

Jan 1, 1967

By James A. Wasson

The Mitchell and Berea sands were cored and logged in Fred Link well K-l, Lower Newport field, Washington County, Ohio. Core and reservoir fluid analyses and available field data were studied to determine if these sands could be successfully waterflooded. The results of the study indicate that there is insufficient oil in place to form an oilbank in either the western Mitchell pool or the Berea sand, and that no commercial recovery of oil by waterflooding can be obtained in these reservoirs.

Jan 1, 1967

By Robert H. Merrill

This Bureau of Mines report summarizes the design and tests of a gage that will simultaneously measure the deformation of a borehole along three diameters 60 degrees apart; the measurements are in a single plane normal to the axis of the borehole. The inherent errors in measurement are considered together with the problems associated with the use of the gage in the relatively severe environments in and around mine openings. These problems were treated in the design and tests of the gage and the results establish that the gage can be used to satisfactorily is determine estimates of the stresses in rock.

Jan 1, 1967