Search Documents

By Robert F. Stewart

The oxidation of structural materials at high temperatures in gas-cooled systems can be greatly retarded by the addition of small amounts of hydrogen to the inert coolant. In experimental equipment for gasifying coal with heat transferred by helium, the oxidation of graphite and metals (molybdenum, tungsten, and certain stainless steels) by trace impurities in the coolant helium was virtually eliminated by adding 0.1 to 1.0 percent hydrogen. The reaction of hydrogen with praphite does not preclude its use to retard oxidation; at 2,400° F. only 0.2 pound of graphite per square foot per year is lost for each percent of hydrogen in the helium. The addition of hydrogen appeared to prevent the mass transfer of carbon often associated with oxidation of graphite, without causing noticeable embrittlement of stainless steels and molybdenum or other damaging effects. This method has been tested in precision gas-recycle systems and applied successfully for more than a year in a pilot-scale unit operating at 250 pounds per square inch gage and 2,400° F. It is now used routinely and can be applied to many gas-cooled systems operating at high temperatures.

Jan 1, 1962

By E. G. King

As low-temperature heat-capacity and entropy data were available for only one sesquisulfide (cerium sesquisulfide), it appeared desirable to augment the information for this class of compounds by measuring the sulfides of antimony and indium. In addition a pressing need existed for data on indium sulfide to supplement vaporization studies in progress in the Department of Mineral Technology, University of California. This Bureau of Mines paper reports low-temperature heat-capacity measurements and entropy evaluations at 298.15° R. of antimony sesquisulfide of stoiehiometric composition (Sb2S3) and of indium sesquisulfide which was somewhat deficient in sulfur (In2S2.93). The data for the latter substance were adjusted to correspond to the stoichiome tric composition (In2S3 ) . Indium sesquisulfide has a lower entropy at 298.15' K, than either antimony sesquisulfide or cerium sesquisulfide, in line with the higher atomic density of the indium compound.

Jan 1, 1962

By Harry R. Nicholls

The objectives of this investigation were to determine the strain propagation laws for a strain pulse in salt and to compare the seismic effects from the detonation of different explosives in salt. The investigation showed that a strain propagation law of the type, e = K(R/W 1/3 ) n, and a strain energy propagation law of the type, Ea/W 1/3 = K(R/WI/3)b , are valid in salt. A change in the regression law coefficient, n , was noted with strain level. A similar change in b was inferred because strain energy is proportional to the square of strain amplitude. Particle velocity data may be used interchangeably with strain data under the test conditions.

Jan 1, 1962

By Oliver C. Fursman

These investigations were conducted to determine conditions for recovery of nickel and copper from Funter Bay, Alaska, sulfide ore and recovery of nickel from nickel-silicate ore, Nickel Mountain, Riddle, Oreg. Samples of Funter Bay cupriferous and nickeliferous pyrrhotite ore, were treated by beneficiation, roasting, electric smelting of roasted are for matte production, chlorination, leaching, and sulfatizing roasting with subsequent leaching. Funter Bay and Nickel Mountain ores were smelted together to produce matte. Total sulfide flotation, followed by magnetic separation of the tailings to recover entrained nickel-bearing pyrrhotite, resulted in the highest nickel recovery in beneficiation tests on Funter Bay are. Overall beneficiation resulted in recovery of 98.5 percent of the copper and 95.4 percent of the nickel in the concentrate that contained 3.5 percent copper and 1.7 percent nickel.

Jan 1, 1962

By K. E. Tame

The Bureau of Mines is studying possible modifications in conventional uranium ore-processing steps to confine and permit controlled disposal of radioactive wastes. A potential method of minimizing pollution from radio-active nuclides, principally radium 226, in uranium mill waste streams is to reuse the waste solutions within the mill. Such reuse of waste solution in the Kerr-McGee Shiprock-type process was investigated in the laboratory. The Shiprock mill employs a two-stage acid-leaching process for dissolution of the uranium, countercurrent decantation for liquid-solid separation and washing, and organophosphorus solvent extraction for recovery of the uranium and vanadium from solution. The simulated use of barren raffinate instead of fresh water in the mill circuit was carried through a laboratory campaign of 28 interlocked leaching, washing, and solvent extraction cycles. About 99 percent of the uranium and 91 percent of the vanadium were dissolved from the are, Washing efficiency in the thickener circuit averaged about 99.5 percent when the pulp was washed with enough barren raffinate and makeup water to recover 2.5 tons of pregnant solution per ton of ore. The only solution discarded was that contained in the washed and thickened leach residue. A buildup of salts due to recycling of solutions did not adversely affect operation of the washing circuit.

Jan 1, 1962

By H. P. LeVan

The aced for reliable reserves of the essential element, manganese, has been a continuing concern of the Federal Government for more than three decades. Because of the increasing vulnerability of outside sources of supply efforts have been intensified to find a means for beneficiating United States domestic deposits. The deposits of most interest would of necessity be near, or have access to, suitable transportation to processing plants. The Georgia manganiferous iron deposits represent some 10 million tons4 of ore readily available to southern iron and steel industries, if a manganese recovery process capable of functioning in the presence of large quantities of iron can be developed. In addition, a successful method for beneficiating the Georgia ore could produce a significant quantity of high-grade iron concentrate. The Differential sulfatization process developed 47 the Bureau of Mines5 seemed to be well suited for this application, particularly because it results in low concentrations of iron in the leach liquors with relatively complete extractions of manganese. In this process, manganese in the presence of iron is preferentially reacted with sulfur dioxide at elevated temperatures and subsequently extracted with water.

Jan 1, 1962

By A. Gene Collins

Potassium, lithium, strontium, barium, and manganese are present in many oilfield brines, None of them except barium is determined routinely in brine analyses. Therefore, sensitive and accurate flame-spectrophotometric methods were developed. Potassium, lithium, and strontium were determined by a standard-addition technique in ethyl alcohol solutions. Barium and manganese were determined in ethyl alcohol and normal propyl solutions, respectively, after interfering substances were removed.

Jan 1, 1962

By E. G. King

The literature contains little thermodynamic information regarding inter-oxidic compounds of the ferroalloy elements and, as a result, thermodynamic considerations of extractive and utilization processes involving these elements have been hampered. As part of a Bureau of Mines program to improve this situation, this paper reports the heats of formation of three calcium vanadates and two magnesium vanadates. There were no previous similar data for any of these compounds. The experimental method was hydrochloric acid solution calorimetry, using calorimetric reaction schemes involving the vanadates and their component oxides. The results were expressed as heats of formation from the component oxides and from the elements. Corresponding free energy of formation values were calculated. The data show that the calcium and magnesium vanadates are stable with respect to all possible decompositions in which vanadium remains pentavalent. This conclusion is similar to the one drawn by Koehler6 for three sodium vanadates.

Jan 1, 1962

By J. L. Potter

An inert-gas fusion technique was applied by the Bureau of Mines to the oxygen analysis of mixed-fluoride electrolytes used in electrowinning uranium and the rare-earth metals. Method development included: (1) Thermodynamic and experimental evaluation of the temperature required to quantitatively remove oxygen from a fluoride melt; (2) installation of a water and an acid trap to entrain the volatilized fluorides; (3) development of a suitable sample-preparation technique for the heterogeneous fluoride baths in which both pulverizing and pelletizing were necessary to achieve reproducible results; (4) comparison of platinum flux and dry crucible techniques, which showed that the use of platinum was not necessary. The accuracy of the method was evaluated by analyzing fluoride baths containing known amounts of oxygen added as the metal oxide. In the 0.05-to 0.5-percent range, the relative error was about ±5 percent.

Jan 1, 1962

By Michael G. Zabetakis

The spillage of liquid diethyl ether in rooms at floor level and 3 feet above the floor resulted in flammable vapor-air mixtures in the immediate vicinity of the exposed liquido The liquid temperature was found to decrease by as much as 35° C., with a resultant decrease in vaporization rate. A search of the literature yielded numerous references to unstable peroxide (residue) formed by the autoxidation of ether. Such residues appear to constitute an explosion hazard in the condensed state.

Jan 1, 1962

By J. G. Donaldson

Optimum conditions are given for chloridizing pyrite, marcasite, chalcopyrite, arsenopyrite, stibnite, and covellite with chlorine gas. The formation of metal chlorides is affected by the time and temperature of chloridizing, and by particle size of the sample. Chloridizing data also are given for chemically precipitated antimony (III) sulfide and copper (II) sulfide.

Jan 1, 1962

By Leonard Obert

This report presents evidence indicating that when rock is stress-relieved during the course of mining or in drilling a core, it may be altered or damaged to the extent that the physical properties of the relieved specimen are not the same as those of the in situ rock. Furthermore, this type of damage may result from stress change other than that accompanying stress relief, such as the application of a relatively large compressive stress. In some instances the damage is microscopic, manifesting itself as incipient cracks or the failure of individual crystal bonds. However, if the sample is taken from a high-stress area, macroscopic damage may occur.

Jan 1, 1962

By M. R. Geer

Information on the performance of coal-cleaning equipment is necessary to provide a basis for evaluating the performance of existing plants and projecting that of new plants. Performance data can contribute greatly to the wise selection and effective use of coal-washing equipment. The Bureau of Mines has published information on the performance of several commercial plants, as well as of some laboratory-scale equipment, 5 (2-9, 11, 12, 17-12, 21-25) from time to time for a number of years. A more intensive program to provide such information for all the principal types of cleaning equipment is underway. The present evaluation of table performance is part of this program.

Jan 1, 1962

By W. W. Agey

The Bureau of Mines examined and tested the rhodonite deposits of the Silverton lead-zinc district, San Juan County, Colo., as a possible source of domestic manganese. Exploration and development work by several mining companies and preliminary reconnaissance of the area by Bureau of Mines engineers indicated the presence of extensive manganese resources in the form of rhodonite. This report summarizes the results of laboratory beneficiation tests made on samples of different type and grade material obtained from surface and underground exposures of seven veins in the district. Surface and underground examinations revealed the presence of several prominent veins that could be traced up to 2 miles for a single vein along the surface. The principal veins average about 50 feet in width and apparently carry rhodonite to considerable depth. Underground samples were taken from the Sunnyside, Silver Queen, Washington, Independence, and Scotia veins. Samples also were taken from surface exposures of the Sunnyside Extension and Hidden Treasure veins.

Jan 1, 1962

By W. L. Dare

Tri-axial strains in pillars, created by pillar robbing, were measured in an experiment at the Dysart No. 1 uranium mine near Grants) New Mexico. At this mine, room-and-pillar stoping is used on the advance, and pillars are recovered on the retreat. The are deposit is, for all practical purposes, horizontal. Measuring devices were installed in pillars approximately 90 to 200 feet from the break line, and strains were recorded over a 4-to 6-week period. The measurements indicate that, in general, the algebraic magnitude of vertical strains increased, and the horizontal strains decreased, in turn, indicating that vertical (or near vertical) loads on the instrumented pillars lessened as pillars were recovered.

Jan 1, 1962

By John J. S. Sebastian

A laboratory-scale investigation was made of the basic problems involved in developing a ceramic heat exchanger to operate at high temperatures for using nuclear heat from gas-cooled process-heat reactors. Technical data were obtained on transferring heat by forced-convection from helium to air in a single-tube vitreous-alumina heat exchanger. Coolant air was passed through the annulus parallel with, and either concurrently or counter to, the flow of helium inside the tube. The data obtained pertain to removing heat from the helium. Average inside film coefficients were determined at mean surface temperatures of 200° to 1,570° F., inlet-gas temperatures of 1,450° to 2,665° F., and Reynolds numbers up to 560. The gas-to-surface temperature ratios were varied from 1.05 to 7.6. The tabulated results are shown in the appendix at the end of this report. The film coefficients of heat transfer were correlated by taking into account the physical properties of the helium at the average fluid temperature. With experimental conditions pointing to a laminar flow, the Nusselt number was found to decrease as the ratio of gas-to-wall temperature was increased to a value of 3. However, within the range tested, gas-to-wall temperature ratios above 3 did not affect the Nusselt number, regardless of the value of the Graetz number. Thus, beyond this point any increase in this ratio ceased to influence the heat-transfer relationship.

Jan 1, 1962

By Michael G. Zabetakis

Limits of flammability of normal propyl nitrate (NPN) vapor were investigated at ambient and elevated temperatures. Minimum spontaneous ignition and decomposition temperatures were determined with laboratory apparatus over the pressure range from 0 to 4,000 p.s.i.g. Flame speeds and the detonation susceptibility of NPN vapor were measured at elevated temperatures. Stable detonation was obtained with liquid NPN at elevated temperatures, and the detonation velocity was determined to be between 4,700 and 5,100 m./sec.

Jan 1, 1962

By E. R. Palowitch

Two samples of the Lower Hartshorne (Spadra) bed were collected: A sample of the raw coal with the machine cuttings excluded, and a sample of the machine cuttings exclusively. Analysis of the 5-inch by 200-mesh size fraction of the raw coal, excluding machine cuttings, showed that a product meeting minimum quality specifications could be produced by washing at 1.60 specific gravity, yielding a theoretical 93.7 percent of clean coal. A negligible amount of near-gravity material at the separation gravity indicated an easy washing problem. The sample of machine cuttings had a maximum size of 2 inches and contained about 50 percent ash. Washability tests of the 2-inch by 200-mesh size fraction indicated that a theoretical yield of 30.0 percent of specification-grade coal could be achieved by washing at 1.49 specific gravity. As the machine cuttings represent an estimated 10 percent of the total coal mined, their inclusion in the mine output would increase the theoretical net yield of salable coal by only 3.7 percent. Because the machine cuttings contained a high percentage of sink 1.80 specific-gravity material, they had neither an effect on the separating gravity required to clean the raw coal nor on the difficulty of separation. Gabbing underground versus transporting the cut-tings to the surface for disposal or washing either separately or combined with the raw coal involves a number of practical, economic; and intangible factors; hence, no specific recommendations could be made. A discussion of some of the factors involved in dealing with a similar problem is given by Gandrud and Riley.4

Jan 1, 1962

By Roy L. Wilfong

The thermal decomposition of the ammonium sulfate, carbonate, nitrate, oxalate, and sulfate salts of praseodymium, neodymium, and samarium was investigated thermogravimetrically in the temperature range 25° to 1,500° C. Each salt was decomposed at a heating rate of 2.5° C, per minute. The pyrolytic sequences have been identified and the temperatures of formation of inter-mediates, the minimum oxide formation temperatures, and values for loss on ignition have been determined. The nonstoichiometric ranges between Pr6011 and Pr203 and the extent of these ranges have been determined for oxides derived from the carbonate, nitrate, and oxalate salts of praseodymium. The alum and sulfate salts of praseodymium produced the sesquioxide without forming the intermediate non-stoichiometric oxides. The temperature limits of formation and regions of stability for the alums and sulfates were better defined than were those for the carbonates, nitrates, and oxalates. The minimum oxide formation temperature increased in the order of samarium, neodymium, and praseodymium irrespective of the anion.

Jan 1, 1962

By H. C. Fuller

Rhodonite, a manganese silicate, occurs as an important component of extensive veins in the San Juan district of Colorado. Recent work by the Bureau of Mines has demonstrated that typical ores of the area can be upgraded to about 30-percent manganese content. Because of their siliceous nature, such concentrates require further processing to convert the manganese into more usable forms. The investigation described in this report demonstrates the technical feasibility of producing silicomanganese from a rhodonitic concentrate by electric smelting methods. The rhodonitic concentrate used in the smelting research was prepared by dry high-intensity magnetic separation of ore from the Silver Queen vein. The concentrate contained 29 percent manganese, 2 percent iron, and 41 percent silica. The principal minerals in the concentrate were 35 percent rhodonite, 30 percent rhodochrosite, and 25 percent quartz and chalcedony. Limestone was used as the flux and coal was used as the reductant. These minerals were crushed and screened to minus 1/2-inch plus la-mesh size.

Jan 1, 1962