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By K. K. Kershner

To meet an increasing demand for high-purity cobalt, the Bureau of Mines has conducted investigations for producing this metal. Cobalt having a purity of 99.95 percent or higher is needed to determine heats of formation, corrosion resistances, phase diagrams, and other basic properties of the element and its compounds. This grade of cobalt may be used for preparing radioactive metal. As a result of its investigations a detailed procedure, which is of practical significance to the production of high-purity cobalt, has been developed by the Bureau for purifying cobalt solutions and for electrolytic deposition of the metal. Cobalt metal, which had a purity of 99.99 percent with reference to metallic contaminations, was deposited electrolytically. Qualitative spectrographic analysis showed only traces of calcium, copper, iron, magnesium, nickel, and zinc.

Jan 1, 1956

By M. M. Wong

Salt mixtures consisting of KC1, BaC12, and HfCl4 with RbCl or CsCl were investigated as electrolytes for refining hafnium. The presence of RbCI or CsCl in the electrolyte appeared to suppress the volatility of. Best electrorefining was obtained with an electrolyte containing 50.7 percent KCl, 27.l percent BaCl2, 15.7 percent CsCl, and 6.5 percent HfCl4. In this electrolyte, hafnium metal with an average oxygen content of 470 ppm was produced from an anode feed containing l,600 ppm oxygen. All metallic impurities were lowered, except titanium, manganese, and tin.

Jan 1, 1966

By B. J. Scheiner

Extraction of silver from silver mill tailings by an electrolytic oxidation procedure was investigated by the Bureau of Mines. Various parameters affecting silver extraction, such as electrolysis time, particle size, and dissolution of the silver as the tetrachloro or cyanide complex, were studied at 30° C with an electrolyte concentration of 20 weight-percent sodium chloride. Resulting silver extractions ranged from 77 to 90 percent, depending on the tailings being treated. Concomitant extraction of mercury ranged between 90 and 95 percent. Power consumption was 52 to 90 kilowatt-hours per ton for the tailings investigated. Comparative experiments using direct cyanidation resulted in extraction of 46 to 82 percent of the silver and 20 percent of the mercury. Cyanide consumption ranged from 3.3 to 9.4 pounds per ton of tailings, depending on the tailings being treated. Silver and mercury were recovered from leach solutions by precipitation on iron powder, followed by conventional distillation and fire refining steps.

Jan 1, 1972

By M. H. Kline

The Chestatee mine is one of several well known pyrite deposits in Georgia that are reputed to carry appreciable quantities of copper with the ore. The deposit is? in Lumpkin County on the Chestatee River, 6 miles northeast of Dahlonega (fig. 1). Old records and reports indicated the probable existence of an extensive unmined ore body, but the mine is inaccessible at present. The Bureau of Mines, after studying old maps and records, decided to cor8-drill along the strike of the lense beyond the limits of the indicated old workings in an attempt to extend the possible reserves. The advantageous location of the property indicates that it could become an economic source of pyrite to be used for the manufacture of sulfuric acid. Iron sinter resulting from the roasting of the ores could be sold at a premium in the Birmingham, Ala., area, and the copper content could be extracted to help replace the nation's depleted resources of this metal.

Jan 1, 1949

By J. D. Ramsdell

The study described in this report was undertaken to obtain information on the character and effect of antimony additions to titanium. The availability of high-purity, low-hardness titanium metal, resulting from fused-salt electrorefining techniques, permitted a reassessment and evaluation of the physical behavior of titanium-antimony alloys. Alloys, based on several grades of titanium containing up to 10 percent antimony, were arc-melted and processed to sheet by hot and cold rolling. Properties and characteristics were evaluated by hardness tests, hot and cold rollability, annealing treatments, metallographic examination, and tensile tests.

Jan 1, 1960

By Aner W. Erickson

Magnetite iron deposits on Tolstoi Mountain were examined as part of the investigations by the Bureau of Mines of iron and copper ores on Prince of Wales Island. The Tolstoi Mountain project was a part of a program for investigating mineral deposits in Alaska, under the general supervision of R. S. Sanford, acting branch chief.

Jan 1, 1948

By G. W. Marks, A. H. Roberson

"Previous investigation 4/ has demonstrated that some of the aliphatic amines are suitable absorbents for 302, This paper reports the results of physical studies of a number of such amines with the object of determining which is most favorable as an absorbent.Monoethanol amine, diethylene triamine, and triethylene tetramine appear to be the most promising of all the amines studied, and most of this report has been devoted to studies of the physical properties of their aqueous solutions, which contain varying amounts of SO2.PURITY OF MATERIALSAll of the amines used were of commercial grade, because the primary object of this research was the investigation of a proposed works process rather than the accumulation of scientific data.The aminoethyl derivitives of ethylene diamine, namely, diethylene triamine, triethylene tetramine, and tetraethylene pentamine, only recently have been produced commercially. The chemistry of aliphatic amines is complex, and these newer derivitives have not been investigated, completely. Chemically pure material is not on the market, and since definite physical standards have not been published, one could not be assured of a pure product even if the commercial material was refined.The compilation of physical constants for the pure amines would involve much time—consuming effort without materially enhancing the value of this paper, as this work was not devoted to the development of fundamental standards."

Oct 1, 1938

By R. V. Ramani, W. Miola

"A relationship exists between the quartz contents in the underground coal nine airborne dust samples and those in the coal and host rocks that are mined [17, 18, 19] The prescribed method for quartz analysis in respirable airborne coal dust samples is the MSHA P-7 method. Accurate quartz analysis procedures are needed for bulk samples in order to predict the potential quartz content in airborne nine dust, which in turn will aid the design of quartz dust control procedures during mining. thereby reducing the airborne quartz dust in underground atmospheres. The requirements of this method are that the amount of quartz is the sample be less than 250ug, and the total sample weight less than 2,500 ug. Unlike with airborne dust samples, there are no limitations to the available mass of bulk samples. However, these are no standard procedures for the preparation of bulk samples for scanning or prescribed methods for quartz analysis. The NIOSH and MSHA methods are certified for roped* dust and the acceptance of these methods for bulk samples assumes that the bulk samples will be reduced to the conditions specified for respirable dust samples. An alternative method is X-ray diffraction, which provides higher average quartz values than those obtained from P-7 method for the same samples.An investigation was carried out to determine the optimal procedure for preparing the bulk samples for the IR and XRD analyses. In this paper, the investigations on the effects of calibration, particle sizes, matrix composition, interferrous, and behavior of the filter substances on IR, XRD and FTIR results are presented. The error introduced by the presence of kaolinite and a new sample asking procedure to reduce it are discussed. The problems experienced with conventional sample holders for scanning were eliminated with the design and development of a new hollow sample holder. Quantitative comparison of quartz determinations by IR, XRD and MR methods on coal, roof and floor rocks, and airborne dust samples are presented. The important factors affecting the results of quartz analysis methods are: 1) bulk sample preparation for obtaining representative and homogeneous analysis samples: 2) particle size distributions of the analysis samples and calibration standards; 3) qualitative matrix composition of the analysis sample; 4) matching calibration standards to analysis sample; 5) substrates for sample deposition during analysis sample preparation; 6) procedures for analysis sample mounting; 7) selection of proper portions of she response profile for insanity measurement; and 8) interferences of spurious phases with the critical analyses. The recommendations of this study are important to enable comparisons and interpretations of analysis and research results."

Nov 1, 1995

By P. J. Colbassani

Samples of mine atmospheres collected by Federal coal-mine inspectors during their inspections and investigations of coal mines, in accordance with provisions of the Federal Coal Mine Safety Act (66 Stat. 692; 30 U. S. C., sees. 451-483) are analyzed routinely by chemical methods at Bureau of Mines laboratories. When samples collected in open workings of nongassy coal mines at points not less than 12 inches from the roof, face, or rib contain 0.25 percent or more methane, the act requires the operator, during operation of such mine, to comply with the provisions of sec. 209, Title II, of the act, which pertain to gassy mines. The methane con-tents of such samples are determined by a physical method based on infrared absorption spectrometry to provide an independent check on analytical results obtained by chemical methods. This information circular describes the equipment and procedures used by the Bureau for determining low concentrations of methane in coal mine atmospheres by infrared absorption spectrometry. ACKNOWLEDGMENTS The authors are indebted to Dr. R. A. Friedel, Chief of Spectrometric Section, Branch of Coal-to-Oil Research, Bureau of Mines, for suggesting the analytical method and for furnishing valuable advice and assistance, and to J. A. Queiser of his staff for making exploratory measurements by this method; to Dr. M. G. Zabetakis of the Division of Explosives Technology for his assistance during the conduct of preliminary experimentation; and to L. B. Berger, Chief, Branch of Health Research, under whose guidance the equipment was procured and the work conducted.

Jan 1, 1958

By Kenneth M. Earl

In its investigation of deposits of strategic minerals, the Bureau of Mines did some diamond drilling at the Almedia deposit In an endeavor to find an additional source of supply of lead and zinc. It is reported that in 1816, lead and zinc minerals were found in the limestone quarries near the boundary line between Scott and Center townships. In an attempt to develop these minerals in paying quantities, an alit was driven for several rods into a bluff Just west of the present Almedia mine, This is believed to be the Web mine, mentioned briefly by Parker Cleaveland in 1816. In 1901 the Almedia mine was developed by an open cut and three shafts. The hoisting shaft at the time of drilling by the Bureau of Mines was sounded to a depth of 115 feet. A concentrating plant reportedly made shipments to Hamburg, Germany, for reduction. The deposit is in a somewhat slaty limestone. The ore occurs in a northeast fracture zone along the strike of the limestone and dips to the southeast. Old miners state that the ore appeared as large chunks of galena and sphalerite. In 1949, to investigate the downward extension of the oreshoot, the Bureau of Mines drilled four holes aggregating 1,126.3 feet.

Jan 1, 1950

By James S. Browning, W. H. Eddy

Laboratory batch and small - scale continuous flotation tests were conducted on a ferruginous barite - fluorspar ore from near Sweetwater , Tenn . , to determine the feasibility of producing commercial - grade fluorspar and barite concentrates . The lignin sulfonate - sodium fluoride - fatty acid method of floating fluorspar produced acid - grade concentrates . Flotation of the barite from the fluorspar tailing using petroleum sulfonate yielded concentrates suitable for use as a weighting agent in oil -well drilling muds . The continuous flotation tests , treating about 150 pounds of ore per hour , yielded fluorspar concentrates that assayed 98.3 percent CaF2 and barite concentrates that assayed 91.2 percent BaSO4 . The recovery of the two minerals was 91.2 and 85.2 percent , respectively .

Jan 1, 1964

By W. W. Adams

"A recent paper prepared by the writer summarized the results of an analysis of the accident records of 34 metal mines for the calendar year 1925. The present paper summarizes the results of a similar analysis of the accident records of 59 coal mines for the same year. This summary is based upon reports furnished to the Bureau of Mines, Department of Commerce, by operating companies that par¬ticipated in the National Safety Competition of 1925.The purpose of the Competition was to establish the lowest accident-severity rate, thus showing the smallest loss of time from accidents in proportion to total number of man-hours worked. The reports covered all lost-time accidents that occurred during the year, that is, all accidents that disabled an employee beyond the day or shift on which the accident occurred. Detailed information for each of the 59 coal mines is given in the appended table. Each mine employed at least fifty men underground; over half of than employed more than 200 men underground. Hence the accident records should be typical of those of large-scale mining operations in general where the company is devoting special attention to accident-prevention work. The mines covered by the reports are situated in eleven States: Alabama, Illinois, Indiana, Kentucky, Maryland, Ohio, Pennsylvania, Tennessee, Utah, Washington, and West Virginia.A tabulation of the reports covering the 59 mines showed an accident-frequency rate of 123 per million hours of ""exposure* and an accident-severity rate of 10.214 per thousand hours of exposure3. The total volume of exposure or employment was 29,117,561 hours, representing the equivalent of work of 12,000 men for three hundred 8-hour shifts. The records covered employment and accident above ground as well as underground, although they did not include stripping or open-pit mining. Accidents during the year resulted in 33 deaths, 1 permanent total disability, 28 permanent partial disabilities, and 3,510 temporary injuries. These accidents represented a loss of tine equal to 297,417 man days. In arriving at this lost-time equivalent, each fatality and permanent total disability was weighted at 6,000 lost days (see footnote 3), as specified in the scale adopted by the International Association of Industrial Accident Boards and Commissions; permanent partial disabilities were weighted according to nature of injury, in accordance with the scale adopted by the :Board; temporary injuries were weighted according to the actual number of calendar days during which the employee was incapacitated as a result of the injury."

Nov 1, 1926

By O. M. Bishop

From October 1943 to March 1944, the Bureau of Mines conducted core drilling at the Victory fluorspar mine, Hardin County, Ill. to test the Fredonia limestone and the included sub-Rosiclare sandstone zone beneath the existing stopes. Twenty-one vertical holes were drilled to an average depth of 60 feet. Ore was penetrated in six holes. Since its discovery in 1927, the Victory mine has produced approximately 5 percent of the total fluorspar mined in the United states after that date. The ore discovered in the early mine development is now exhausted, except that contained in pillars drifting to the northeast has partly developed one substantial ore body, and company drilling has indicated another nearby. The increasing need for fluorite for war use in 1943 suggested the desirability of mining the pillars, provided it could be established that no ore beds existed below the stopes or in areas to which access would be obtained through the present workings. This work describes the work accomplished during the project and presents the data obtained.

Jan 1, 1948

By E. C. Lane

Although motor gasoline marketed in the United States in January of this year was, on the average, slightly more volatile than that sold in January 1925, the improvement in quality is too small to be of importance. In other words, there is no evidence that any radical change in the quality of gasoline is being made at the present time. During the past six years the Bureau of Mines has made semi-annual surveys of the gasoline marketed in the United States, the survey just completed being the thirteenth in the series. The cities in which samples have been collected have been chosen as representative of the more important marketing territories as it is obviously impracticable to obtain a sample of every gasoline sold in the entire country.

Jan 1, 1926

By Victor E. Kral

"SUMMARYFollowing a magnetometer survey on the McCoy iron deposit, a trenching and drilling program was carried out by the Bureau of Mines in August 1944.This deposit is 32.3 miles southwest of Battle Mountain in the McCoy Mining District, Lander County, Nevada, and lies on the east flank of the Fish Creek Mountains at an altitude of 5,400 feet, about 1 1/2 miles south of the gold camp of McCoy.Total production from the deposit has been 400 tons of magnetite, mined by hand and shipped to the west coast for ship's ballast.Bureau drilled two holes to a total depth of 92 feet and excavated 12 feet of trenches. Both holes were drilled in the same ore body and engineered magnetite ore 14 and 11 feet thick. Trenching was used successfully to show the lateral limits of the ore.Magnetite ore bodies were found to occur as replacements of a limestone bed in quartzite. They outcrop near and parallel to the exposure of a diorite entrusting that forms a long westward-trending ridge. Although magnetic outcrops can be traced for 5,000 feet trenching definitely proved the ore bodies to be disconnected to have little or no lateral extent beyond their outcrops. Only two ore bodies more than 10 feet thick were found; one of these is the inaccessible to and the other was drilled by the Bureau."

Jan 1, 1947

By Constantine C. Popoff

During 1946 several limestone deposits near Fortson, Snohomish County, Wash., were examined by the Bureau of Mines. These examinations were part of a long-range investigative program of regional mineral supplies required by the anticipated industrial development of the Pacific Northwest. The .study outlined in the following paper was specifically undertaken to disclose new sources of high-purity limestone and to appraise, their economic aspects. The deposits examined -namely the Galbraith, Climax, and Hi, Hi -are somewhat similar in physical features and geologic environment. They are lenticular and belong to the same formation of metamorphosed sediments that underlies the prominent Whitehorse Ridge.

Jan 1, 1949

By H. S. Caldwell

The objective of this investigation by the Bureau of Mines was to develop and test for laboratory use a retort embodying many features required for practical commercial-scale applications of vacuum distillation of metals. A gas-fired vacuum retort was developed comprising a hollow, cylindrical graphite liner encased in a thin shell of stainless steel. The liner prevents the shell from collapsing under vacuum and protects it from corrosion by metal vapors and the molten metal charge. The vacuum-tight shell protects the liner from oxidation and flame erosion. The retort was used to distill zinc from dross and die-casting scrap. More than 99 percent of the zinc was recovered as a condensate containing 99.8 to 99.9 percent zinc. (Atmospheric distillation recovers 95 to 98 percent at a purity of 99.5 percent zinc.) Distillation rates of 50 pounds of zinc per hour were attained at a temperature of 65° C. with pressures ranging between 50 and 100 microns. Distillation at this low temperature is not practicable at atmospheric pressure. Also, the retort is suitable for distilling other volatile metals such as cadmium and magnesium.

Jan 1, 1961

By Homer J. Ballinger

The Rex mine is one of several zinc deposits in Ozark and Howell Counties, Mo. It is the second of these deposits investigated by the Bureau of Mines in an effort to demonstrate reserves of sulfide ore underlying the shallow carbonate ores from which the district's major production has come. The initial investigation was made during 1945-46 on the Alice mine, Ozark County, Mo.21 The investigation reported herein was conducted during 1947. The Rex open pit is about 250 feet long, 100 feet wide, and about 25 feet deep (average). Three caved shafts are evident in the bottom of the pit, but the extent of the workings from these shafts is not known. The Bureau of Mines drilled five churn-drill holes in and around the Rex pit to test the grade and the vertical and lateral extent of the deposit. Two of the holes indicate notable zinc mineralization ranging from less than 1 to more than 10 percent metallic zinc, but largely in the oxidized condition.

Jan 1, 1948

By N. S. Dalal, Xiaoya Sun, Xianglin Shi

"The in vivo toxicity of vanadium(V) has been found to correlate with the depletion of cellular glutathione and related non-protein thiols. With a view to understanding the mechanism for this observation, we have investigated the oxidation of glutathione, cysteine N·acetylcystcinc and pcnicil· lamine by vanadium(V), using electron spin resonance (ESR) and ESR spin trapping methodology. The spin trap used was 5,5-dimethyl-l-pyrroline I-oxide (DMPO). It is found that the oxidation of these thiols by vanadium(V) generates the corresponding thiyl radicals and vanadilim- (IV) complexes. The results suggest that free radical reactions play a significant role in the depletion of cellular thiols by vanadium(V) and hence in vanadium(V) toxicity. 1. INTRODUCTIONThis communication reports on the identification of thiyl radicals formed as intermediates in the reaction of vanadium(V) with glutathione (GSH) and related nonprotein thiols. This study was undertaken because the biochemical mechanism of vanadium toxicity is still not fully understood,. despite being a topic of current research activity [1-20). As to possible clues, it is known that vanadium is most toxic when administered in its pentavaient state [21), and that vanadium(V) administration into laboratory mice reduces cellular levels of NAD(P)H and GSH [22). While the oxidation of NAD(P)H by vanadium has been studied extensively [16-20), that of glutathione and related non-protein thiols has been paid less attention. On the other hand, GSH and related thiols are important cellular antioxidants [23). Their functions include decomposing lipid peroxides and protecting cell membranes [23-25). Thus any reduction in the cellular contents of such nonprotein thiols after vanadium exposure may result in the accumulation of lipid peroxides which might ultimately lead to tissue injury. With a view of finding the mechanism for this thiol depletion process, we have investigated reactions of non-protein thiols with vanadium(V). Particular attention has been paid to the detection of thiyl radicals, since it has been postulated [l] (but not experimentally proven) that the glutathionyl radical (GS·) might be an intermediate in the reaction between vanadium(V), NADH and GSH. We have used electron spin resonance (ESR) and ESR spin trapping methodology for investigating the reactions of GSH, cysteine, N-acetylcysteine and penicillamine with vanadium(V). The results show that the corresponding thiyl radicals are indeed formed in the one-electron reduction of vanadium(V) by all of the above mentioned thiols."

Jan 1, 1990

By N. S. Dalal, X. Shi

"Electron spin resonance measurements provide evidence for the formation of long-lived Cr(V) intermediates in the reduction of Cr(Vl) by glutathione redtuctase in the presence of NADPH and for the hydroxyl radical formation during the glutathione reductase catalyzed reduction of Cr(Vl). Hydrogen peroxide suppresses Cr(V) and enhances the formation of hydroxyl radicals. Thus Cr(V) intermediates catalyze generation of hydroxyl radicals from hydrogen peroxide through a Fenton-like reaction. Thus the mechanism of Cr(VI) toxicity might involve the interaction between macromolecules and the hydroxyl radicals.C(Vl) compounds have been found to exert serious toxic and carcinogenic effects on humans and animals (1-3). In contrast, most Cr(III) compounds are relatively nontoxic, noncarcinogenic, and nonmutagenic (1,4). Cr(VI) and Cr(III) oxidation states are different in their metabolic pathways: Cr(VI) , ions are rapidly transported across cellular membrane (1,4,5), while Cr[III) moieties do not easily penetrate cells and are not oxidized by cellular constituents (!). Since it is known that the reduction of Cr(VI) ion is required for its reaction with DNA (1), the molecular mechanisms for the intracellular Cr(Vl) reduction has been the focus of current studies but the details are still not understood.Earlier studies on the mechanism of Cr(Vl) reduction include those on the reduction of Cr(VIJ by glutathione (GSH) .0,6-8), ascorbic acid (9), glucose (10), lactose (IO), galacturonic acid (11), microsome (12), and mitochondrial electron transport chain complexes (13). These studies have shown that the Cr(VI) reduction involves the formation of Cr(V)-containing species which are often considered to be the toxic form of chromium. Thus far, however, no information is· available on the subsequent fate of those biologically formed Cr(V) species, in particular employing well defined biochemical systems. In this context, we report here our investigations of the reduction of Cr(VI) by glutathione reductase (GSSG-R). This enzyme was selected because it is ubiquitously present in cellular systems and it has been postulated to be involved in the Cr(VI) reduction (14-17) but the underlying mechanism has not been clarified. We find that the reduction proces·s involves not only Cr(V) but also ·OH radicals. We further investigate the reactivity of Cr(V) and find that it catalyzes generation of OH radical from H2O 2 through a Fenton-like reaction. The role of ·OH in Cr(VI) carcinogenicity is suggested from this study."

Jan 1, 1989