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By S. L. May

The Bureau of Mines has developed several methods for extracting tantalum and columbium (niobium) and the rare-earth compounds from ores and concentrates. A cooperative agreement was made by the Bureau with Porter Bros. Corporation of Idaho to process 200 pounds of its euxenite concentrate by methods that had been developed at the Albany, Oreg., Metallurgy Research Center. The euxenite concentrate was processed to extract and purify the valuable metals by chlorination, solvent extraction, and hydrometallurgical techniques. Chlorination was used to convert the valuable constituents into chlorides and to partly separate them. Solvent extraction techniques were used to separate the tantalum from the columbium. The rare-earth and uranium compounds were purified by hydrometallurgical methods.

Jan 1, 1959

By E. S. Longfellow, S. H. Katz

Poisonous hydrocyanic acid gas (HCN) is sometimes evolved in dangerous quantities from cyanides used in metallurgical and chemical operations. This gas is much used for fumigating buildings, ships, greenhouses, and such commodities as grain and cotton to destroy rats, mice and insect pests. Wherever cyanide fumes are evolved, thorough ventilation is necessary in order to render the sur- rounding air safe to breathe. Many persons have been killed by entering tanks and fumigated places too soon, and a simple test for this gas would promote safety. In view of the need for an easy method for quantitatively determining HCN in air, the three color reactions used originally for testing HCN in solution tions *** were modified and adapted. The reactions employ (1) picric acid (CH(NO2)3OH) which is yellow but combines with hydrogen cyanide to form a red- purple dye, isopurpuric acid****; (2) phenolphthalin (CH1604), which is a reduc- tian product of the phenolphthalein (CH4) used for acid indicator, this colorless substance is oxidized***** by presence of HCN to pink colored phenolph- thalin; and (3) guaiacum which oxidized from colorless to blue******. Phenolph- thalin and guaiacum require the presence of copper compounds which catalize the color formation by reduction of cupric cyanide. The chemical processes involved *Associate physical organic chemist, Bureau of Mines, Department of the Interior. **Assistant gas chemist, Bureau of Mines, Department of the Interior. 2014 20 *** Kohn-Abrest, E., Notice toxicologique sur les gas: Arnales des Falsifica- tions, vol. 8, 1915, pp. 215-35. (Tested air with picric acid and guaiacum papers). **** Élasiwietz, H., Ueber eine neue Zersetzungsweise der Trinitrophenylsaure: Anal. der Chemie, vol. 110, 1859, pp. 289-303. ***** Weehuizen, F., Phenolphthalin as reagent for HCN: Pharmaceutrisch weekblad, Utrecht, vol. 42, 1905, pp. 271-2. Abstract, Jour. Chem. Soc., vol. 88, part 2, 1905, p. 489. ****** Schonbein, C. F., Ueber den thatigen Zustand der Helfte des in dem Kupfer- oxydenthaltenen Sauerstoffs und ein darauf beruhendes hochst empfindliches Reagens auf die Blausaure und die loslichen Cyanmetalle: Jour. fur. Praktische Chemie, vol. 106, 1869, pp. 263-70.

Jun 1, 1923

By J. R. Hauger, P. A. Romans, W. J. Niebuhr

With suitable instrumentation and techniques it is possible to determine the presence of tantalum in columbium to 20 ppm . This paper discusses the selection of X- ray spectrographic instrumentation and describes a technique for accomplishing the low level determination of tantalum . An ion- exchange method of separating tantalum from columbium is also described .

Jan 1, 1964

By D. J. MacDonald

This U.S. Bureau of Mines report reviews published information on synthetic berlinite (AlP04) and suggests experimental conditions requisite for its production. Berlinite is a piezoelectric material with potential use as a substitute for quartz in the crystal oscillators, which are components of electronic and electroacoustic equipment. Information gathered here (mostly from published sources) includes historical background, physical properties, end-use applications, criteria of quality, and physio-chemical factors involved in berlinite crystal growth. It is concluded that growing large high-quality berlinite crystal would require high-purity starting materials in an autoclave equipped with a noncorrodible liner and operated with temperature control of ±O.OO5 ac over a range of 250 to 350 ac.

Jan 1, 1995

By D. W. Dareing

Multiple branch wellbores and horizontal holes, when applied to deep lying ore bodies, have the potential of significantly reducing well costs by reducing total footage drilled per acre of well pattern. In addition, horizontal holes may increase sweep efficiency. Well completion is a major problem. They must be cased to contain leaching solutions within the underground portion of the production loop. Several drilling and completion concepts are given and evaluated in the report. Our evaluation shows that there is economic incentive to further develop these concepts for field application to ore bodies 1,500 feet. Multiple branch concepts are the most attractive. They can reduce well costs by as much as 30° when applied to 2,000 feet ore body depths (44%, at 5,000 feet) and can accommodate a lamer pump than conventional vertical wells. We recommend this concept be developed further to accommodate either dual or triple branches.

Jan 1, 1980

By James P. Bennett

The Bureau of Mines investigated the effect of refractory oxide additions, introduced in soluble form, on the high-temperature properties of 90- and 98-pct-MgO brick. Brick samples were soaked in solutions containing Al, Ca, Cr, Co, Fe, Mg, Mn, Mo, Ni, Si, Sr, Sn, Ti, or Zr ions. Additions to 98-pct-MgO brick did not generally result in statistically significant property improvements. Statistically significant improvements were noted in hot modulus of rupture (MOR), slag resistance, and spalling resistance of the 90-pct-MgO brick for additions of Al, Mg, or Sn. High-temperature performance of treated 90-pct-MgO refractories was equal to or approached that of 98-pct-MgO brick. The marked improvements due to tin were obtained with additions of only 1.14 wt pct Sn02.

Jan 1, 1985

THIS bulletin presents all analytical and lest methods regularly used by Bureau of Mines laboratories for characterizing coal and coke. To provide better service to coal producers and consumers, the scope of this bulletin has been expanded to include important test methods used to evaluate coal properties for commercial processing. The methods described will prove valuable to all persons interested in analyzing and testing coal and coke.

Jan 1, 1967

By R. O. Dannenberg

This report describes aperiments by the Bureau of Mines and reviews theoretical aspects of the use of organophosphate solvent extraction for recovering beryllium from sulfate leach liquors. The leach liquors were prepared by sulfuric acid leaching of lime-sintered low-tenor beryl flotation concentrates. The experimental work on sulfate leach liquors showed that the acidic esters of organophosphates extracted beryllium slowly but in preference to aluminum. Three common alkylphosphoric acids, di- (2-ethylhexyl) (EHPA), heptadecyl (HDPA), and dodecyl (DDPA), in order of decrmsing selectivity, yielded a partial separation of beryllium from aluminum.

Jan 1, 1962

I do not regard the criticism by Rankin of my work as valid or even meaningful. I strongly reject the assertion by Rankin that my results are invalid. As stated in my paper, the equation to solve (in e. m.u. ) is: [ ] where n2 =4 ps? . This may be rewritten as three scalar equations in Cartesian coordinates, one of which is [ ] The equation to be solved is the diffusion equation, and it is not appropriate to consider waves in this context. In the method a point-wise solution to the problem is approximated. As discussed in my paper the approach taken at discontinuities in conductivity is to choose the normal component of [E] at the discontinuity as the average of the normal components on either side of the discontinuity. This is similar to the well-known assumption made in obtaining Fourier series representations for piecewise continuous functions (Pipes, 1958; p. 51). In the geophysical problem this means that the discontinuity is approximated by a transition zone, which is a very good approximation for such cases. By using this approach, both the values of the function and its derivatives give a good estimate for those associated with the physical situation. It is not apparent and Rankin has not shown that "all the field components and the derivatives are grossly distorted in the region about the boundary" for geophysically realistic situations. He has given no evidence to support his assertation that the results are "invalid". Although Rankin declares that one cannot calculate the electric components from the magnetic, in his discussion he has not stated why this is so. After once calculating the magnetic components the electric components may be calculated, but one must insure that the initial solution is accurate enough to prevent significant round-off errors.

Jan 1, 1973

By Harry K. James

Experimental studies of the physical and explosion characteristics of pure hydrazine nitrate and multicomponent systems containing hydrazine nitrate, supplemented with an extensive Literature survey, are presented. Such proper- ties as melting point, heat of fusion, density, viscosity, surface tension, thermal stability, decomposition process, detonation velocity, impact sensitivity, and TNT equivalence are included.

Jan 1, 1970

By E. G. Davis

The Bureau of Mines made laboratory-scale experiments to examine the technical possibilities of reclaiming manganese from slags produced by oxygen lancing of high-manganese pig iron. Ferromanganese was added to molten pig iron to yield a 4-to 5-percent manganese hot metal, which simulated a product obtainable from the blast furnace. This was injected with oxygen to reduce the metal to 1 percent or less manganese and form a slag containing about 40 percent manganese. The molten slag was water-quenched, treated with H2SO4) roasted at 660° C, and water-leached to give soluble manganese and iron sulfates. The sulfates were precipitated as hydroxides, converted to the oxide form, and smelted to produce a standard ferromanganese containing 74.6 percent Mn and 0.01 percent P. As an alternate method of manganese recovery, a manganese cell feed was prepared from the leach solutions and electrolytic manganese was produced. Direct smelting of the high-manganese slag resulted in 74.2 ferromanganese meeting ASTM specifications except for phosphorus content. The high phosphorus content of the metal and high slag-to-metal ratio obtained made this approach unattractive.

Jan 1, 1966

By W. W. Simpson

The Bureau of Mines conducted research to determine the effects of potassium trithiocarbonate (KTTC), a degradation product of potassium ethylxanthate (KEX), on flotation of chalcopyrite and molybdenite. Small amounts of KTTC were identified in fresh and aged solutions of KEX using thin-layer chromotography. Hallimond tube flotation tests on pure minerals showed that KTTC acts as a weak collector for chalcopyrite. Both KEX and KTTC tend to depress molybdenite, but the depression effect is easily overcome by addition of a small quantity of fuel oil. The results of the Hallimond tube tests were confirmed in batch flotation tests using a porphyry copper ore.

Jan 1, 1983

By Arthur V. Petty

The Bureau of Mines has investigated the effect of refractory oxide additions, introduced in soluble form, on the refractory properties of 42-, 58-, and 70-pct-A1203 brick. Brick having porosities ranging from 12 to 16 pct were impregnated with solutions containing chrome, chrome-iron, zirconium, calcium, magnesium, cobalt, nickel, tin, and manganese ions. Additions of some of these ions provided dramatic improvements to such properties as hot modulus of rupture, hot load, and particularly slag resistance. These improvements can be related to reduction of porosity, amorphous grain boundary phases, formation of more refractory bond phases, and reduction of the wettability of Al203-containing refractories by metallurgical slags. Fifty-eight-percent-AI203 brick, impregnated with chrome, showed hot modulus of rupture, hot load, and slag resistance two to five times better than those of untreated 70-pct-AI203 brick. This could result in reducing the Nation's dependence on imported refractory-grade bauxite generally required for high-A1203 brick, as domestic alumina resouces could be used to produce the improved refractories.

Jan 1, 1984

By H. D. Jacobs

A process for recovering both iron and manganese from four manganiferous ores of the Cuyuna Range was evaluated. It comprised: (1) Low-temperature gaseous reduction to convert nonmagnetic iron minerals to magnetite and manganic minerals to manganous oxide, (2) acid leaching to extract manganese, and (3) magnetic separation to reclaim iron from the leach residue. Iron recoveries from the magnetic products ranged from 70 percent to 90 percent; manganese recoveries from leach filtrates ranged from 75 percent to 95 percent. Two ores, from the Hillcrest and South Alstead properties, yielded magnetic products considered adequate for use as blast furnace feed. Although good yields of manganese were attained on all ores, appreciable iron accompanied the manganese into solution. Previous work, however, has shown that this iron can be precipitated almost quantitatively under autoclave oxygen pressure with very little loss of manganese.

Jan 1, 1970

By R. R. Hornor

Due mainly to conditions brought about by the war , the metal mining industry in this country is now passing through one of the most critical stages in its history , and is confronted by new problems upon the solution and adjustment of which depends , in a large measure , its future welfare and prosperity . The chief factors contributing to the cost of production are the cost of labor and supplies . It is conceded by our leading mine operators , managers , and engineers that any material reduction in the cost of labor or supplies , within possibly the next two or three years , cannot be anticipated , anl it is not thought likely that pre - war prices will ever again prevail . This being true , the mine operator must look in some cther direction to effect economies that will lower production costs . If this cannot be accomplished it will mean , in many instances , that mines and metallurgical works will have to be closed and abandoned , which will tend to disorganize the entire industry . How to lower production costs and still maintain the present high standard of wage , is the problem that is engaging the serious attention of mine operators and managers over the entire country . In As a solution to this problem it is thought that the most promising field of investigation lies in the direction of systematizing and standardizing mining practice , so as to effect economies in the use of both labor and materials . other words , to eliminate , in so far as possible , unproductive effort and waste and thereby secure a maximum of productive results , It is not the idea to speed up work or to demand a greater effort on the part of the workman , but rather so to systematize and standardize the various under ground operations that his energy will be directed into more useful and productive channels ,

Dec 1, 1919

By Thomas C. Mowatt

Chemical and petrographic studies were carried out on selected tin-bearing rock samples of contact-metasomatic origin from the Cassiterite Creek and Brooks Mountain areas, Seward Peninsula, Alaska. The tin content of rocks ranged from 0.39 to 8.9 pct. Leaching with a 20 pct hydrochloric acid solution released from 19.3 to 67.9 pct of the tin. Cassiterite was not observed in the rock samples. These results are significant with regard to tin recovery and reserve delineation in these and similar occurrences. Part of this leachable tin may be associated with metasomatic borate minerals.

Jan 1, 2011

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 Wilbert T. Malenka

In its search for a highly productive mining system for anthracite beds pitching from 100 to 200, where conventional mobile equipment cannot be used) the Bureau initiated a longwall project by introducing a shearer drum cutter loader of European origin. Because of the undulating nature of the roof and floor and changing bed thicknesses, the machine proved inflexible and extra work was required in lifting bottom coal and blasting top coal.

Jan 1, 1966

By R. M. Creamer

Attempts have been made to electroplate titanium and zirconium from aqueous, nonaqueous, and fused-salt electrolytes. Metals were produced only in fused-salt electrolytes, the major product being sponge metal. All other electrolytes gave only partial reduction of the metal ions. Fused alkali borate electrolytes containing titanium salts gave titanium boride powders and coatings of poor adherence. Some of the problems encountered in the deposition of these metals and some of the aspects of titanium and zirconium chemistry involved are discussed. INTRODUCTION Titanium and zirconium are both relatively light, noncorrosive metals with both military and civilian uses. This has led to intensive investigations into the metallurgy of these metals. Both metals are high in the Electrochemical Displacement Series and are difficult to prepare in a pure state. At present they are prepared by reducing their chlorides, using magnesium. Electrolytic reductions have resulted in the preparation of fine powders or sponge of variable quality. It is believed that a good process of electroplating these metals on a baser metal would result in a very desirable product. The objective of the research summarized in this report was to investigate methods of electrodepositing these metals, with the idea of producing uniform, coherent plates. Most of the work was concentrated on titanium, the more abundant of the two metals. A system developed for titanium should be applicable to zirconium owing to their chemical similarity. Information gained from these experiments may also be applicable to the electro-winning of the metal.

Jan 1, 1954

By Benjamin W. Haynes

This research was conducted as part of the U.S. Department of the Interior, Bureau of Mines program to recover metals, glass, and a combustible fraction from municipal solid waste (MSW). The objective of this analytical study was to determine the concentration of antimony, arsenic, and mercury in samples taken from various sampling areas in the Bureau of Mines raw refuse recycling plant and to compare these values with those for coals used in the generation of electricity. To provide the necessary analytical data, sensitive reproducible ashing-chemical digestion-atomic absorption procedures were adapted from published procedures. It was determined that antimony and mercury concentrations in the combustible fraction of MSW are approximately an order of magnitude higher than those found in coals presently used for power generation;' the arsenic concentration is similar in both fuels.

Jan 1, 1978