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By Harry Freund, Kenneth H. Hammill, Francis C. Bissonnette

"Gallic acid is a sensitive, stable, colorimetric reagent for the determination of tantalum in the range of 2 to 40 µ g.Ta/ml. The method consists of the fusion of tantalum oxide with potassium pyrosulfate and solution of the cooled melt in saturated ammonium oxalate, followed by development of a yellow complex with an ethanolic solution of gallic acid. The tantalum-gallic acid complex absorbs over a broad region in the blue and near ultraviolet. Adverse effects due to interfering ions and solution conditions, such as oxalate concentration and pH, can be minimized by a suitable choice of wave length.by a suitable choice of wave length.A new and sensitive colorimetric method is provided that has been used successfully at the Northwest Electrodevelopment Laboratory of the Federal Bureau of Mines for determining minor amounts of tantalum.INTRODUCTIONThe development of corrosion-resistant alloys at the Northwest Electrodevelopment Laboratory prompted a review of the analytical chemistry of columbium (niobium) and tantahnn. Not only are these elements difficult to determine in small amounts, but tantalum especially lacks both sensitive and characteristic color reactions. Various phenolic compounds have been suggested as colorimetric reagents for tantalum, Quentin and Wagner (10, p. 24B) 1/ recommend the use of tannin. The use of pyrogallol was suggested originally by Krivoshlykov (6, pp. 59-60), whose method recently has been subject to a number of modifications (3, pp. 249-254; 5, pp. 1340-1344; 1, pp. 1803-18oi; 4, pp. 345-350). The yellow coloration produced by pyrocatechol in an oxalate solution containing tantalum may also be used to estimate tantalum ( 11, pp, ll-1-4-148) . The use of hydrogen peroxide has been recommended also (7, pp. 164-165; 9, pp. 926-931).Aside from a lack of specificity and sensitivity, the major failing of phenolic reagents is their susceptibility to air oxidation. The oxidation products are highly colored and absorb in the same spectral region as the tantalum complex. Holding reductants are not completely satisfactory in minimizing this effect. Increasing the acidity, while retarding the oxidation, has an adverse effect on the tantalum sensitivity."

Sep 1, 1956

By George T. Faust

The petrographic microscope plays an important role in the mineral dressing of nonmetallic materials. Petrographers and mineral technologists have evinced an interest in the technique developed, specifically, for mineral-dressing problems. The following dissertation makes the informa¬tion more generally available. ACKNOWLEDGMENTS The authors are indebted to O. C. Ralston, chief engineer, Nonmetals Division, and to Will H. Coghill, supervising engineer of the Southern Experiment Station for a critical reading of the manuscript. They are also indebted to their colleagues for technical information obtained in the course of cooperative work, in particular to J. B. Clemmer for the use of the data on fluorite.

Jan 1, 1940

By L. D. Schmidt, H. G. Graham

Several processes for the production of ultra-clean coal for electrode carbon were developed in Germany prior to and during World War II . These processes have been investigated since the end of the war by the British and U. S. Government missions . As the reports of the investigations are not readily available to the public , it is the purpose of this paper to present the information which has been obtained regarding the methods by which ultraclean coal was produced . Almost all the ultra-clean coal was used in the manufacture of electrodes for the production of aluminum and magnesium . Standard raw materials for making these electrodes are pitch coke and petroleum coke , which are nearly ashless . The inclusion of ash in the electrode carbon results in lowered efficiency and impure metal from the reduction process . Petroleum coke and pitch coke were in very short supply in Germany during the war , so that it was necessary to augment the supply with carbon produced from coal . In the emergency , methods were developed to clean coal which had never before been economically feasible . However , a demand for nearly ash-free coal might develop in the United States if a shortage of petroleum coke were to occur at the same time as a strong demand for light metals . Other uses of ultraclean coal are in direct hydrogenation of coal , in production of activated carbon, and for special fuels . Specifications for electrode carbon are rather severe owing to the necessity for producing pure metal . Maximum amounts of impurities allowable in American practice are as follows : Total ash , 1.0 percent ( in finished coke , 0.7 percent ) Silica , 0.08 percent Ca or Na, or their sum , 0.12 percent Sulfur , 2.0 percent Ba , Ni , Cr , Mn , Co , and V are objectionable in very small amounts . The most important process for ultra cleaning of coal in Germany was froth flotation . Froth flotation had been used widely there to process washery -water sludges and to recover coking coal from high - ash fines . Its use was indicated , therefore , when the demand for ultra low-ash coal arose . In two plants the coal cleaned by froth flotation was treated with acid or caustic to lower further the ash content . Another process used on an industrial scale was that of dissolving the coal substance in the middle oil from direct hydrogenation of coal under controlled pressure and temperature . The resulting paste was heated, filtered , and the oil distilled off . The residue was a low-ash organic material that could be carbonized for electrode carbon or could be hydrogenated directly . Several other processes had been developed to the laboratory or pilot - plant stage but had never been used on a commercial scale . These processes included cleaning by centrifugal action , cleaning by electrostatic action , and cleaning by forming a paste with oil in water . The coal-preparation plants at the Carl Alexander mine , Augusta Viktoria mine , and Kőenigin Elisabeth mine are described in Bureau of Mines Information Circular 7389 : " Coal Preparation Practice in Western Germany" , by Thomas . Fraser and M. G. Driessen . Most of the special equipment used at these plants is described in the above publication .

Oct 1, 1948

By Tell Ertl, Ernest E. Burgh, John R. Wagner

The principal goal of the Oil-Shale Mining Division is to develop the most economical methods and practices for mining oil shale. Experimental work in the mine has not progressed far enough to conduct full-scale breaking tests; therefore, mining season - to October 31, 1945, has been confined largely to problems connected with drilling cost oil shale. Calculations have indicated that commercial production will result in breaking the oil shale; the largest individual turn will be for drilling. This paper is a report on the progress of phase two of drilling research to date; it outlines the development of a successful hard-surfaced rock bit for drilling oil shale.

Dec 1, 1948

By Joseph Berman

The wolframite mineral series was studied to determine the effect of the FeO - MnO ratio on unit cell symmetry and thermal stability. This work was undertaken to evaluate the analytical procedures now in use for wolframite in scheelite and to aid in the development of improved methods of analysis. Wolframite grains were hand-picked, crushed, and screened; impurities were removed by selective magnetic separations using a Frantz isodynamic separator. The samples were further checked by optical spectroscopic and microscopic examination.

Jan 1, 1957

By D. A. Wilson

A laboratory method for processing lead battery scrap has been developed that eliminates virtually all of the S02 emission that normally is produced when a reverberatory or blast furnace is used. The method employs a hydrometallurgical step to convert the PbS04 to PbO and CaS04 by mixing the battery scrap with a slurry of Ca(OH)2. The reaction is exothermic and goes to completion in 2 to 5 minutes at room temperature. The dried product is mixed with a KC1-NaC1 flux and carbon and reduced at 6500 C. A minimum charge ratio of 3 parts of carbon to 100 parts of battery scrap is required for reduction. The process produces lead reductions and recoveries as high as 97.0 and 94.9 percent, respectively. The KCI-NaCl flux is recovered using a standard counter-current water leach followed by evaporation.

Jan 1, 1976

By T. M. Barczak

One of the primary goals of Bureau of Mines research is to reduce the cost of coal mining by improving the efficiency of longwall supports. One method of achieving this goal is the optimization of stress distribution within the support structure, resulting in a lower overall weight, more fully stressed shield. However, before stress optimization can be initiated, load conditions must be defined that cause maximum stress in the various support components. A finite-element model of a longwall shield was used to identify these critical load conditions. These load conditions were then evaluated in the Bureau's mine roof simulator (MRS) by instrumentation of a longwall shield and measurement of strains in each of the shield components. The critical (canopy-base contact) load conditions were identified that can cause structural failure at less than rated shield (hydraulic yield) capacity. Comparisons were made between full-contact and partial-contact load conditions. Other parameters investigated included the stiffness of the contact material, changes in shield geometry, rate of load application, and effects of horizontal constraint. Conclusions were drawn regarding the structural integrity of the major shield components and potential for stress optimization.

Jan 1, 1987

By Floyd G. Anderson

The increasing trend toward use of continuous-type mining machines created a significant dust problem in coal mining, which resolved itself into three categories: Visibility at face, deposition on return airways, and the potential health hazard. The control measures applicable to these conditions and studied or developed from 1955 through 1957 are summarized and reviewed in this report. Other important problems brought into focus during the same period were radiation exposure in uranium mining and high temperature and humidity. Although temperature and atmospheric pressure alone may not be contributing factors in the incidence of silicosis, the few mining companies who operate under the extremes of these conditions are dust conscious and keep dust-control engineers on their operating staffs.

Jan 1, 1961

By P. J. McDonough

The Bureau of Mines designed and tested a hardware-software system for measuring on-line corrosion rates of materials in a rod mill in operation. Currents ranging from 10-6 to 10-3 A and potentials in I-mV increments were converted to a digital signal. The digitized data were frequency-modulated and transmitted from a rotating ball mill to an FM receiver, where they were decoded by computer and then processed in real time using assembly language software. This design approach would allow accurate measurement and control of systems where signals of small amplitude and large ranges are present.

Jan 1, 1988

By R. H. Jefferson

An electrochemical method to selectively determine sulfur dioxide in the presence of sulfur trioxide was investigated. A hydrophobic gas-permeable membrane separates the gas sample solution from an internal filling solution containing a fixed quantity of chloride ion and a sufficiently large excess of sodium bisulfite so that its concentration may be considered constant. Sulfur dioxide diffuses through the membrane to dissolve in the internal filling solution and liberates an equivalent quantity of hydrogen ions. The electromotive force between a precision-ground, flat-ended pH electrode, which acts as the sensing element, and a chloride sensing electrode, which acts as the reference element, gives a direct measure of S02 in the gas sample solution. Calibration curves in water, tetrachloromercurate (TCM) , and citrate buffer absorption solutions were closely parallel with slopes in their linear segments, ranging from 57 to 52 mv/decade of S02 concentration. The slopes compare reasonably well with the theoretically expected slope of 58 millivolts at 21° C. The water standard curve was linear with respect to the logarithm of S02 concentration from 1 to 1,000 ppm S02; the TCM standard curve was linear from 10 to 2,000 ppm S02; and the citrate standard curve was linear from 30 to 5,000 ppm S02' The high efficiency and nontoxicity of citrate favor it as a substitute for the conventionally used TCM in the absorption solution.

Jan 1, 1976

By G. L. Neumann

The Guymard mine in Orange County, N. Y., is reported to have been discovered in 1862 and mined until 1876, producing 10,000 tons of lead and zinc ore. The property was examined by an engineer of the Bureau of Mines in 1948. Development work was done by the Bureau in April and May 1949 and March 1950. During these two periods four drill holes totaling 2,090 feet were completed. The mineralized sections of the core were sampled and assayed.

Jan 1, 1952

By R. L. Benner

A compound stability diagram was constructed by the Bureau of Mines for the Zn-Fe-S-O system to show the phases that should be thermodynamically stable at various temperatures, oxygen pressures, and SO2 pressures. The diagram was demonstrated to have good qualitative value for predicting stable phases that may, in turn, be related to the recovery of zinc in the leaching phase of the electrolytic zinc process. The study showed that roasting temperature is the most Significant variable in preventing roaster formation of zinc ferrite, which is directly related to subsequent extraction of zinc in the leaching step.

Jan 1, 1966

By A. W. Fahrenwald

As an aid to studies of grinding, a batch laboratory classifier and elutriator has been developed at the U. S. Bureau of Mines Metallurgical Field Office at Moscow, Idaho, in cooperation with the University of Idaho. It is designed for use in conjunction with other batch laboratory apparatus, such as ball mills and flotation machines. It is shown in Figure 1. Description and Operation of Batch Laboratory Classifier The classifying column is a cylinder 4 feet 2 inches long, of 5 3/4-inch inside diameter, and terminates at its top in a cone or funnel 18 inches in diameter at the overflow elevation. The pressure chamber is of the same diameter as the classifying column, and has a conical bottom; it is provided with two openings, one in the cylindrical portion through which water is admitted, and the other, a small drain hole, in the apex of the conical bottom. The two compartments are bolted together and communicate with each other through the medium of a constriction plate provided with 3/16-inch holes spaced 1/2 inch apart. Constriction plates having any other percentage of opening may be substituted as the needs demand water is admitted to the compartment below the constriction plate at constant pressure. The volume of eater admitted is controlled with a valve. It should be mentioned that the classifying column at the bottom, just above the constriction plate, is glass.

Jan 1, 1929

By T. A. Sullivan

High-purity vanadium metal was prepared by electrorefining commercial vanadium in a molten sodium bromide, potassium bromide, and vanadium dibromide electrolyte. Variables investigated were operating temperature, current densities, electrolyte composition, and condition of the anode. The purity of the refined metal was in the range of 99.95 percent vana-dium. Iron and oxygen in the 50- to 250-ppm range were the only major impurities. Metal with hardness numbers of 50 to 60 in the Rockwell F scale was prepared from feed material with a Rockwell B hardness of 90. The arc-melted metal was highly ductile and could be cold-worked into sheet or foil.

Jan 1, 1965

By D. Harrington

More or less unconsciously and from sheer force of habit human beings do many things they probably would not do if the possible consequences of their acts were fully recognized and appreciated. Such carelessness ordinarily could be condoned if human life were not at stake, but it is difficult to understand why intelligent men engaged in the hazardous occupation of mining indulge with the utmost indifference in some habit or continue some custom in violation of State leas and company regulations and under circumstances that may jeopardize not only their own lives but those of scores, even of hundreds, of their fellow workers as well. The old adage that stolen sweets are the best may or nay not have some foundation, but when applied to the practice of smoking surreptitiously in a coal mine, more especially a gassy mine, it is without even remote justification. Although a relatively harmless habit in the proper environment, smoking has been the cause or suspected cause of many gas explosions and black-powder ignitions and has resulted in numerous instances of bodily injury, loss of life, and destruction of property. Likewise, many fires in both coal and metal nines, causing loss of life, have been started by smoking.

Jan 1, 1941

By John W. Walkiewicz

The U.S. Bureau of Mines has conducted studies to utilize rapid microwave heating to stress fracture ore samples. Iron ores containing hematite, magnetite, and goethite were subjected to microwave energy in batch operations at 3 kW and heated to average maximum temperatures between 840 and 940 °C. Standard Bond grindability tests showed that microwave heating reduced the work index of iron ores by 10 to 24 pct. In a microwave chamber designed to simulate a continuous throughput operation at 3 kW, the grindability of a taconite ore was improved by 13 pct at a bulk temperature of 197 °C. Because stress cracking occurred at a lower temperature, less energy was consumed. To further improve the economics of microwave fracturing, higher powers up to 16 kW were used to rapidly heat samples to relatively low temperatures in a continuous, belt-fed applicator. A significant improvement of grindability was obtained with a larger rod mill feed size in comparison to a minus 6-mesh Bond feed.

Jan 1, 2010

By M. R. Geer

American and European practices in cleaning fine coal are strikingly different. The tables, launders, classifiers, and pneumatic devices used in America are seldom employed in Continental Europe, where much of the fine coal is cleaned in feldspar jigs, often supplemented by froth flotation of the extreme fines. This difference in choice of cleaning equipment may be fortuitous, but in large measure can be attributed to a difference in economic factors. Coal being more costly in Europe, there is greater emphasis on efficient cleaning of all sizes, including the extreme fines, and it is common to produce a high-ash middling for "on-site" consumption to avoid any waste of fuel value. The feldspar jig has been found advantageous under these conditions. In the United States fuel coal must be prepared as cheaply as possible, and metallurgical coal must be prepared as efficiently as possible; thus in both branches of preparation practice, any cleaning device that promises greater economy or higher efficiency warrants consideration. The feldspar jig, as employed in Europe, has a much higher unit capacity than the wet table used so extensively here and therefore offers economy in the capital costs of a washery through saving in space. As pointed out by Vissac,4/ the jig operates under automatic control, and therefore can cope with fluctuations in quality of feed. Maintenance costs for a single, large-capacity unit, such as the feldspar jig, would be expected to be lower than those for a battery of low-capacity cleaners. These considerations led the Bureau of Mines to undertake an investigation of the feldspar jig to determine its possible usefulness in this country.

Jan 1, 1958

By Sam S. Taylor, H. M. Smith

"INTRODUCTION In most oil fields, natural gas is the major source of energy causing flow of oil to the well. The amount of gas Produced with the oil generally exceeds actual energy requirements, so that in time the gas reserve of the field becomes seriously depleted and the oil production must be stimulated by some auxiliary means. One of these is to repressure the oil formation with natural gas; or, where a gas supply is not available, often air is used.Although P.ir is a Cheap and convenient repressuring medium, its use sometimes is attended with several disadvantages. First, the return air-gas mixture decreases rapidly in fuel value, often until it can be used no longer as a source of power. At the same time, explosive mixtures may result if recycling is used, causing hazards to life and equipment. Second, some fields experience considerable trouble with the formation of emulsions which become increasingly difficult to treat. Although there is no definite proof that air repressuring always causes these emulsions, many operators are convinced that this is the case. The Petroleum Experiment Station of the United States Bureau of Mines at Bartlesville, Okla., has been interested in problems connected with air-repressuring for a number of years. Some time was spent in studying the so-called ""bad gas""--return,mixture of low fuel value. However, it appeared impossible to attack the problem successfully from this angle, and an approach was made through a laboratory--scale study of direct oxidation of crude oil."

May 1, 1934

By John J. Mulligan

Since 1941 the Federal Bureau of Mines has been conducting an intermit-tent program of placer and lode investigations to evaluate the potential tin resources of the western Seward Peninsula tin belt. Previous investigations were made in the Potato, Cape, Brooks (Lost River), and Ear Mountain areas. As part of this program the Bureau made a reconnaissance of reportedly tin-bearing stream gravels in areas adjacent to the previously worked tin deposits at Lost River and Potato Mountain. The objective of the reconnaissance was to determine if additional areas might be favorable for lode or placer exploration. The work was begun late in the fall of 1956 and completed during the following summer. The streams sampled were the Lost River and York Creek in the Brooks Mountain area and the Anikovik River and Kigezruk and Baituk Creeks in the York area. Samples were obtained by churn-drilling methods employing conventional placer-evaluation procedures. Holes were drilled at wide intervals at sites chosen as being representative of drainage areas rather than of individual gravel deposits. Minor to trace amounts of tin were found in the gravels of all these streams, but the highest grade was 0.35 pound of tin per cubic yard in the gravels of Lost River below the mouth of Tin Creek. Small amounts of gold were found on Baituk Creek and in one hole on the Anikovik River; the highest grade did not exceed 10 cents per cubic yard. Traces of scheelite and barite were found on York Creek, chromite was encountered in one hole on the Anikovik River, and minor amounts of titanium minerals (probably derived from basaltic intrusives) were found in the York area.

Jan 1, 1959

By F. S. Wartman

The presence of magnetite, either dissolved or suspended as solid crystals, in slags from the copper reverberatory furnace is a frequently mentioned cause of an abnormally high copper content in those slags. The presence of this oxide in the slag is to be expected, since it is present in appreciable amounts in both converter slag and roaster calcine which comprise a considerable proportion of the furnace feed. Magnetite is also a product of some of the furnace reactions. These abnormal losses result in several ways. Magnetite is supposed to favor the formation and retention of copper ferrite, in the slag. Crystals of solid magnetite suspended in the slag are objectionable-because they make the slag less fluid and often entrap globules of matte. Frequently these crystals settle into a layer at the slab-matte interface which may have such mechanical strength as to create a false bottom and interfere with furnace operation by preventing separation of matte from slag. Magnetite may, by crystallizing on the furnace bottom, build the bottom to such a level that the furnace can no longer be operated.

Jan 1, 1928