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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 Theodore M. Katz, W. Stephen Brightwell, David E. LeGrande, Joseph J. Hurrell, Jane A. Lipscomb, Nancy Lessin, Lawrence R. Murphy, Michael J. Colligan, Steven L. Sauter, Richard A. Lippin

Revolutionary changes in the organization of work have far outpaced our knowledge about the implications of these changes for the quality of working life and for safety and health on the job. This gap in knowledge is one of the 21 priority areas for research under the National Occupational Research Agenda (NORA)—a framework crafted by the National Institute for Occupational Safety and Health (NIOSH) and its partners to guide research into the next decade. This report was developed under NORA as the first attempt to develop a comprehensive research agenda for investigating and reducing occupational safety and health risks associated with the changing organization of work. Research and development needs identified in the agenda include (1) improved surveillance mechanisms to better track how the organization of work is changing, (2) accelerated research on safety and health implications of the changing organization of work, (3) increased research focus on organizational interventions to protect safety and health, and (4) steps to formalize and nurture organization of work as a distinctive field in occupational safety and health.

Jan 4, 2002

By Timothy A. Clancy

In support of research on forming ceramics from mining and processing wastes, the Bureau of Mines tested various commercial refractories to evaluate their resistance to melts of these wastes. Sixteen refractories of various types were exposed in slag erosion tests to two siliceous waste melts with Si02/CaO ratios of 4.0 and 2.2, The extent and nature of slag attack were then determined for each refractory. The nature of slag attack was investigated through scanning electron micrographs and microprobe elemental distributions. The refractories that performed best in resisting attack by the melts were high-alumina types, and of the refractories tested, the most resistant was a 90-pct-Al203, 10-pct-Cr203 refractory.

Jan 1, 1983

By E. G. King

Heat of formation values for mercuric sulfide appear in all the comprehensive listings of thermodynamic data, but experimentally determined entropy values have been lacking. Consequently, all free energy calculations involving mercuric sulfide have been based upon estimated entropy values. This paper reports Bureau of Mines measurements of the low-temperature heat capacity of red mercuric sulfide (cinnabar) and the entropy value at 298.15° K. derived therefrom. The entropy value was combined with heat data to obtain free energy values for the formation of red mercuric sulfide from liquid or gaseous mercury and from rhombic or gaseous diatomic sulfur.

Jan 1, 1962

Develop hydrometallurgical or pyrometallurgical recycling methods to recover valuable rare-earth compounds from various forms of NdFeB magnet scrap. Background The U.S. Bureau of Mines (USBM) has developed technology to treat and recycle a variety of wastes containing valuable and strategic metals. As part of this effort, the USBM developed a process to separate neodymium and other valuable rare earths from iron in NdFeB magnet scrap (fig. 1). Since this scrap typically contains nearly 30 weight percent neodymium and since the demand for neodymium is constantly increasing, cost-effective methods for scrap treatment could have a significant impact on industrial expenditure and materials supply in the expanding area of magnet manufacture. Approach A hydromctallurgical, H2SO4 dissolution-precipitation process provided the most effective treatment for separating rare earths from bulk NdFcB magnet scrap (fig. 2). Precipitation of neodymium-alkali sulfate double salt proved advantageous over direct precipitation of fluoride or oxalate products. This double salt is easily converted to a variety of useful rare-earth compounds, which eliminates many of the materials-handling and economic problems inherent with direct precipitation. Following rare-earth precipitation, dissolved iron was removed from the acid leach solution by precipitation as a jarosite.

Jan 1, 1993

By Charles R. Harrison

The purpose of this study and resulting development of the training program, "Safety--Let's Make It Happen" was to determine the relation of concepts to the development of desired Health and Safety behavior. After extensive pre-contract study, it was hypothesized that improved acceptance and understanding of the Federal Coal Mine Health and Safety Act of 1969 could possibly contribute to the reduction of accidents. Second, in order for an individual to accept and understand the Act, he or she must have a working knowledge of its purposes and application. Third, acceptance and understanding of the Act, necessary to protect the individual from negligence, was imperative. Fourth, an actual operating company could provide the base in which to test these hypotheses in a meaningful manner and develop this type of training program. Six assumptions were agreed upon before embarking on this study and training program development. (1) In the cognitive process, a concept introduction into an individual's personality may result in a behavior quite different than if he or she had been exposed to a different concept.

Jan 1, 1977

By R. H. Lien

The Bureau of Mines investigated nitrous oxide (N20) stability when used as a solvent for organic removal from metal powder surfaces. Both supercritical and subcritical conditions were studied. This investigation was prompted by the occurrence of a violent reaction when supercritical N20 was being used to deoil a metal powder grinding waste sample that contained 20 to 25 wt pct cutting oil. Tests were conducted to determine the cause of the reaction and to define stability limits. Test data showed that the waste's oil fraction reacted violently with N20 acting as an oxidizer; the metal powder acted as a promoter to reduce the ignition temperature. Although the data were scattered, this temperature appeared to reach a minimum at a certain pressure (dependent on vessel and sample size). The minimum ignition temperature for a 0.64-g sample in a 72-cm3 vessel was 360° C at 200 psig. As the sample size increased, the ignition temperature decreased. For example, when the sample size was increased to 10 g, a reaction occurred at 240° C and 600 psig. Because of the variability of ignition temperature with pressure and sample size, safe operating conditions were not established. Overall, this research showed that extreme caution should be exercised when using N20 in an organic or organic-metal system.

Jan 1, 2011

By ALICE V. Petar

Like many gem materials, amber has a colorful history which may be traced through the writings of the ancients and the ornamental relics discovered from time to time. Like few gem materials, however, it is distinctly useful in products whose value has no connection with the gem industry. Long prized for its beauty, amber was fashioned into articles of jewelry and ornaments to please the fancy of ancient rulers and to find a place among treasured pos- sessions in their tombs; it has been used by adherents of various creeds for rosaries and other religious symbols; and although still sold for these pur- poses it also lends itself to such commercial purposes as raw material for varnish. Amber is only on the border-line of the mineral kingdom; actually it is of vegetable origin, having been formed as resin from trees of the conifer family that existed during the Tertiary period. It is the hardest of the fos- sil gums. The United States produces no amber, although a few occurrences are known. Most of the world's supply comes from East Prussia, where it is ob- tained from both land and sea. For many years pieces of amber were gathered from the Baltic by fishermen and deep-sea divers; and although about 10 per- cent of the Prussian amber is still recovered from the sea, most of the out- put is mined from open pits on the Samland Peninsula.

Jun 1, 1934

By G. L. Hundley

The Bureau of Mines has devised a procedure to recover chromium chemicals from concentrates derived from low-grade domestic chromites. These domestic chromites contain silicon and aluminum impurities at levels that are too high to permit processing by present industrial processes. The Bureau procedure consists of reacting chromite with molten NaOH under oxidizing conditions to form sodium chromate (Na2Cr04)' The reaction product is leached with methanol to recover the majority of the unreacted NaOH, then with water to extract the Na2Cr04 and the remainder of the NaOH. The Na2Cr04 product is recovered by evaporative crystallization from the aqueous solution. This report presents laboratory results of studies to determine the optimum leaching conditions for the reaction products of several domestic chromite concentrates. Results of solution purification and crystallization studies are also presented. The concentrates are from a variety of sources including the Stillwater Complex in Montana, Red Bluff Bay and the Kenai Peninsula in Alaska, and a Ni-Co laterite from southern Oregon. Sodium chromate crystals were produced that contained less than 0.01 pct NaOH.

Jan 1, 1988

By James R. Boyle

The value of Alabama's nonfuel mineral production in 1986 was $405.2 million, a slight decrease from that of 1985. Alabama was second in the Nation in production of bauxite, crushed marble, and ferroalloys; third b fire clay; fifth in masonry cement and lime; sixth in total clays; and seventh in recovered sulfur. Alabama ranked 19th nationally in value of nonfuel minerals produced. Cement, clays, lime, sand and gravel, and stone were the major commodities produced.

Jan 1, 1988

By A. L. Engel

In the period of 1942-1945, medium-grade, oxidized, lead-silver ore was mined and shipped from the Diamond district near Eureka, Nev. An encouraging tonnage of low-grade ore was developed during these operations and partly blocked-out for future mining. If the low-grade ore could be treated profitably, further development of the district would result, and production of an important strategic metal might be increased. A representative sample of Diamond district ore was obtained through the Reno office of the Mining Division for the studies described in this report. The sample consisted of lumps and fines of a highly altered siliceous rock containing much earthy red hematite and some granular black hematite. Examination with the binocular microscope showed the lead carbonate mineral, cerussite, in seams and disseminated in the hematite. No zinc or silver minerals were identified, and no sulfide minerals were present. Analyses of the ore showed:

Jan 1, 1951

By J. K. Whyatt

The U.S. Bureau of Mines has been conducting a series of rock mechanics investigations at the Lucky Friday Mine in the Coeur d'Alene Mining District of northern Idaho. In the present study, the energy release rate (ERR) index was used to evaluate three underhand stope backfill parameters-cement content, density, and placement gap-to determine their influence on rock bursts. This index provides a relative measure of the likelihood of rock bursting for a given rock mass. It is known that the elastic idealization of the rock mass inherent in this method causes underestimation of stope closure and hence underestimation of the influence of backfill on rock bursting. However, this evaluation still showed that (1) changing from present practice to one in which backfill was omitted altogether would increase the ERR by 42 pct and (2) perfect placement of backfill would reduce the ERR below present practice levels by 28 pct. The easiest step toward perfect placement would be elimination of the placement gap, which accounted for half of the difference in ERR between present practice and ideal placement conditions. There was no indication that increasing initial fill strength through increased cement content would affect the ERR.

Jan 1, 2010

By E. V. Cilento, K. A. DiGregorio, R. C. Lantz

"An electro-optical method was used to quantify superoxide (SO) release from single rat pulmonary alveolar macrophages (PAM) exposed in vitro to respirable quartz and kaolin dusts and in vivo to quartz. Release was determined by measuring the reduction of nitroblue tdrazolium (NBT) to a diformazan precipitate at 550 nm from video-recorded images of individual cells. In vitro exposure to 0.025 or 0.05 mg/ml kaolin for 40 minutes resulted in no significant differences in either the total diformazan produced (max) or the maximum rate of diformazan production (R)./n vitro exposure to 0.025 mg/ml c1uartz decreased max 38 percent while no significant change was found using 0.05 mg/ml. However, R was decreased 31 percent and 24 percent for the low and high dose, respectively. In contrast, PAM obtained from animals exposed in vivo to quartz dust for two or four weeks in inhalation chambers exhibited increased production of diformazan. However, only PAM analyzed three days post-exposure showed significant increases, while PAM from animals sacrificed ten or 31 days post-exposure were not significantly different from control. The combined in vitro and in vivo quartz results might suggest that there is an initital acute response to exposure that decreases the ability of PAM to produce SO, followed by recruitment of production of PAM with increased SO producing capability. It appears that removal of animals from the source of exposure permits PAM to return to control levels of SO production by31 days. Whether this would be true for chronic exposure remains to be elucidated.IntroductionPulmonary alveolar macrophages (PAM) protect the lungs by phagocytizing foreign debris and bacteria.(1) This process involves ingestion as well as destruction of foreign matter. Phagocytosis usually is accompanied by a respiratory burst which increases cellular oxygen consumption leading to the release of highly reactive oxygen metabolites.(2) These agents have been implicated in the killing of bacteria by phagocytes, but they have also been shown to be toxic and,have been linked to cancer, emphysema, arthritis, diabetes, and other diseases.(3) Toxic effects may be a result of 1) an abnormally low production of metabolites, resulting in damage to lung tissue by the respired bacteria and/or dusts; or 2) an abnormally high production resulting in direct damage to lung tissue by metabolites themselves."

Mar 1, 1989

By H. H. Dewing

The U.S. Bureau of Mines characterized Hg-containing wastes and used a thermal-desorption process to remove and recover the contained Hg. The wastes were generated by an electrical-parts plant engaged in the assembly of Hg-containing switches and contained phenolic resins and paper insulating materials mixed with soil. The average Hg content was 396 ppm. Numerous characterization tests showed the Hg was tightly absorbed and could not be removed or concentrated by leaching or gravity separation techniques. Laboratory retort tests showed the Hg content reduced to < 16 ppm in 2 h at 400 °C; rotary-kiln, thermal-desorption tests required 4 h at 450 °C. Airflow through the retort im¬proved thermal-desorption efficiency, but vacuum operation only slightly reduced the temperature needed for thermal desorption. Offgases from decomposition of organic materials were burned in a high-temperature afterburner and subsequently cooled in a heat exchanger to condense water vapor. Finally, the Hg vapor was condensed and absorbed from the offgas by activated charcoal. Mercury recovery was over 99.99 pct of the desorbed Hg. Thermal-desorption processes have had wide application to many Hg-containing wastes, and historical experience in Hg mining has demonstrated its potential cost effectiveness.

Jan 1, 2010

By J. A. Eisele

The Federal Bureau of Mines is engaged in a continuing program on the recovery of alumina from domestic source materials. Of the six processes being studied, current efforts focus on HCl leach of clays. A key step in the HCI process is the removal of iron from the aluminum chloride leach liquor. This was accomplished .by solvent extracting the iron with a tertiary amine in kerosine to which decanol was added as a phase modifier. In a mixer-settler operation, iron in the raffinate was reduced to <10 ppm in two extraction stages from a feed containing 1.4 gil Fe. Iron was stripped from the organic phase in three stages with dilute HCl.

Jan 1, 1976

By C. B. Daellenbach

A prototype particulate size analyzer system was developed that would rapidly determine size distributions of homogeneous and two-mineral materials in the 74-micrometer (200-mesh) to 7-micrometer size range. The system sizes particles in a series of hydrocyclone elutriation steps and senses the weight of the five sized fractions by nuclear attenuation techniques. Size distribution of materials was determined from experimentally developed mathematical relationships that existed between particulate weight and the measured transmittance of gamma rays from an Americium-241 source. In the developmental phases, size distributions of three minerals (quartz, magnetite, and hematite) and a laboratory prepared two-mineral mixture of quartz and magnetite were accurately determined by the prototype system. In later stages of the investigation, semiconcentrates, an intermediate magnetic product from a taconite plant, were evaluated. Using 25-gram feed samples of this industrial material, the analyzer system was found to predict weight percentages for individual size fractions with an accuracy of ±0.85 percent or better at a 95-percent confidence level.

Jan 1, 1974

By James S. Browning

For the past several years, the Bureau of Mines has conducted laboratory and continuous process development work on weathered mica pegmatites and micaceous schist ores to determine the feasibility of recovering commercial-grade mica concentrates by flotation. The research has resulted in the development of two processes for flotadon of mica: an acid cationic method for recovery of coarse mica, and an alkaline anionic-cationic method for recovery of fine mica. The research indicated that the two processes may be effectively utilized separately or in combination for flotation of mica from weathered pegmatites and micaceous schists. Concentrates containing over 98 percent mica, with recoveries ranging from 77 to 92 percent, were obtained from the pegmatite ores. The micaceous schist ores yielded concentrates containing 95 to 98 percent mica, with recoveries ranging from 70 to 83 percent. Part 1 of this report summarizes the process development work and demonstrates the feasibility of producing commercial- grade mica concentrates. The report also includes details of commercial beneficiation and grinding of .mica.

Jan 1, 1973

The objective of this study was two-fold: 1. To perform a world literature search pertinent to the analysis, selection and design of hoisting systems and their components and to codify the search into a literature compendium. The search resulted in a technical data file of over 1500 hard copy items. The compendium index was also suitable for establishing a comprehensive computer-loaded data base on the subject. 2. To develop a comprehensive system of guidelines to cover salient aspects of analysis, selection and design of electrical, mechanical and structural components of a hoisting system with a view to establish parameters for maximum safety and efficiency of operation, installation and revision of the system. 3. Major mechanical components in the hoist and mechanical drive train are considered. Design and specification criteria based on American standards and practices are developed as they apply to typical mine hoist arrangements.

Jan 1, 1988

By John B. Bennett

In this report estimates are presented of the impact of the passage of five recently proposed "acid rain" bills on electric utility costs for coal-burning utilities servicing the domestic aluminum smelting industry, and on the costs of production for affected aluminum smelters. As aluminum smelting is an energy-intensive industry, domestic increases in electricity prices could affect the industry&apos;s competitiveness. Energy costs in U.S. aluminum smelting are compared to aluminum smelting energy costs in the rest-of-the-world. Governmental policies affecting these energy costs are discussed.

Jan 1, 1988

By H. M. Cooper

The determination of moisture in coal is an empirical test, because the time, temperature, and equipment are specified. The essential features of the equipment and details of the procedure are given in A.S.T.M. Designation: D271-44.:2. According to the specifications, the following features should be incorporated in the equipment used: 1. Oven must have uniform temperature in all parts. 2. Oven must be constructed with minimum of air space. 3. Oven must have means of changing the air two to four times per minute. 4. Air must be dried over sulfuric acid (sp. f-7. 1.84). The analytical procedures governing most of the nation&apos;s coal purchases are those given in A.S.T.M. Standards referred to above. These standards are general arid of such scope as to cover all ranks and types of coal. In cases where only the moisture is required, a faster method than the standard procedure is desired.

Jan 1, 1948