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By Benjamin W. Haynes

Analytical procedures are described for the quantitative determination of 16 elements (As, Ba, Be, Cd, Co, Cr, Cu, Fe, Mn, Mo, Ni, Pb, Sb, Se, TI, and Zn) and 7 ionic species (NH4, C032-, CI-, F-, NO3-, P043-, SO42-), identification of major and minor mineral components, and measurement of physical properties associated with manganese nodules and nodule processing reject waste materials. Compound identification methods discussed include X-ray diffraction, infrared spectroscopy, scanning and transmission electron microscopy, selective area electron diffraction, and optical and reflected light microscopy. Methods for elemental analysis include atomic absorption spectrophotometry, inductively coupled plasma emission spectroscopy, neutron activation analysis, fluorescent X-ray spectrography, and ion chromatography. Thermal gravimetric analysis, ultraviolet-visible spectrophotometry, ion specific electrodes, and standard wet chemical procedures are briefly discussed. Physical properties determined in manganese nodule materials include grain size distribution, specific gravity, triaxial shear, permeability, maximum density, Atterberg limits, and slurry density. The results of a round-robin analysis of an ammonia process waste material and manganese nodule standards demonstrate the applicability of the discussed methods. Tests discussed for the evaluation of the waste materials for disposal options include the Environmental Protection Agency (EPA) EP toxicity test, the ASTM shake extraction test, and the U.S. Army Corps of Engineers EPA seawater elutriant test.

Jan 1, 1983

By Gerald W. Elger

This report describes development of the fusion-leach crystallization precipitation process for producing a hafnium content feed material for hafnium-zirconium separation plants. Mixtures of zircon, potassium silicofluoride, and potassium carbonate (or potassium chloride) were fused to prepare soluble potassium zirconium hexafluoride-potassium hafnium hexafluoride salts. High extraction of these salts was obtained by countercurrent leaching the fused material in dilute hydrofluoric acid. About one-half of the hafnium was recovered in hafnium-enriched mother liquor by cooling clarified lead: liquor to crystallize most of the zirconium salt. Additional hafnium was recovered from the primary crystals in a multiple dissolution-recrystallization step. Hafnium-enriched oxides having a hafnium-zirconium ratio of more than three times that of zircon were precipitated from the combined mother liquors. The hafnium and zirconium recoveries in the precipitate were 83 and 24 percent, respectively. About 71 percent of the zirconium and the remainder of the hafnium were recovered in potassium zirconium hexafluoride crystals of low-hafnium content.

Jan 1, 1966

By G. A. Smyres

A GaC12--B2 l-eachtng procedure and meEal-recovery method for treating an arsenical Cu-Co sulfide concentrate was developed by the Bureau of Mines as an alternative to smelting, which is no longer considered an environmentally acceptable method for treating arsenic-containing ores. The procedure involved leaching in a CaC12 solution with CaC03 for 96 h at 26 pct solids (concentrate and CaC03), 1150 C, and a pressure of 50 psig (345 kPa) with oxygen. More than 98 pct of the cobalt and 97 pct of the copper were extracted, and 99.98 pct of the arsenic and 99.9 pct of the iron remained in the leached residue. A filtration rate of 2.9 gal/(ft2.h) [118 L/(m2.h)] and a cake formation rate of 36 Ib/(ft2.h) [172 kg/(m2.h)] were obtained by filtering reacted pulp at 1000 C. More than 99 pct of the copper in the pregnant solution was extracted as CuCl2 by golvent extraction with a new copper extractant. Copper was stripped from the loaded organic with a sulfate-chloride solution, which was used as the anolyte for electrowinning of copper in a membrane cell. Copper plate produced was more than 99.99 pct pure and requi.red 0.81 (kW'h)/lb Cu [1.78 (kW·h)/kg Cu]. Cobalt sulfide was precipitated at pH 3 with Ca(HS)2.

Jan 1, 1986

By Davis E. Traut

TiC14, AIC13, and VC14 were coreduced simultaneously via a Kroll-type magnesium reduction to form an alloy sponge as part of a research effort by the Bureau of Mines to produce titanium alloy powder. Reduction tem-peratures of 750°, 850°, and 950° C, a range of chloride feed rates from 34 to 152 Ib/(ft2·h), and crucible diameters of 7-3/4 and 10-1/4 in were tested. Microprobe analyses using a 40-um-diam spot showed no effect on alloy microhomogeneity (distribution of Al and V in the Ti, considered critical as a powder property), due to changes in process variables within these ranges. Statistical analysis of these data for alloy sponge indicated greater variation in the chemical composition (AI and V) than that found in commercial Ti-6Al-4V plate or Plasma Rotating Electrode Process (PREP) powder. Therefore, a one-step approach to pow-der, such as grinding the Ti alloy sponge, would not produce a powder product of acceptable chemical homogeneity. An approach that homoge-nized the sponge, such as with a melting step, would produce an accept-able powder product with respect to chemical homogeneity.

Jan 1, 1987

By Agnes Y. Lee

The Bureau of Mines has developed an effective hydrometallurgical method to recover high-purity Pb metal and elemental S from concentrates. This low-temperature process eliminates S gases and Pb emissions, in contrast to the current high-temperature smelting technology. The method consists of (1) oxidative leaching with H202, Pb02, and waste fluosilicic acid at 95° C to produce a solution of PbSiF6 and a residue containing elemental S, (2) electrowinning the PbSiF6 solution at 35° C to produce 99.99 pct Pb metal and H2SiF6, and (3) solvent extraction to recover S, leaving a residue containing Cu, Ag, and other metal values. Spent electrolyte was recycled repeatedly, with impurity buildup controlled by controlling the leach parameters.

Jan 1, 1986

By Dean C. Holt

This work was done to appraise the potential of titanium minerals in known titanium- bearing placer deposits and potential titanium- bearing placer areas in western Montana . Reconnaissance studies were made of more than 225 stream areas . Churn drilling and other placer exploration techniques were used in sampling eight deposits . The sampling results indicate that areas containing more than 10 pounds of ilmenite and other titanium- bearing black - sand minerals per cubic yard occur in the Bitterroot , Upper Clark Fork , and Jefferson River drainages . The chief source for the constituents of the black sands appears to be the Idaho batholith , and the highest black - sand concentrations are generally found near the source . Sample testing methods include gravity and magnetic separation and visual microscopic as well as chemical and radiometric analyses on deposits sampled in detail .

Jan 1, 1964

By Valois R. Shea-Albin

Ground control problems are an important factor affecting safety, production, and efficiency in underground coal mines. A major portion of ground control problems encountered in underground coal mines can be attributed to geologic features in the strata surrounding the extracted coal seam. The U.S. Bureau of Mines has compiled information from numerous sources on the geological features that contribute to ground control problems in underground coal mines. The compilation includes (1) sedimentary features such as paleochannels, crevasse splays, clastic dikes, mold-and-cast structures, concretions, and lithologic factors, and (2) structural features such as folds, fractures, joints, cleat, and faults. The compiled information will aid in identifying the features, predicting their occurrence in advance of mining, and controlling or minimizing roof failure when these features are encountered in an underground coal mine.

Jan 1, 1993

By Charles B. Kenahan

The effects of ultrasonic radiation on the electrodeposition of copper-zinc, copper-cadmium, and copper-tin alloys from cyanide baths were investigated by the Bureau of Mines at frequencies of 18.5 and 38 kilocycles per second, and at acoustic intensities up to 0.5 watt per cm3. Significant changes occurred in the composition of the deposited alloys; some of these deposits were brighter, harder, more adherent, or of finer grain size than nonirradiated deposits. The irradiated deposits were also smoother and less porous, and they afforded better corrosion protection for the substrate metal in sodium chloride solution. The limiting current densities of the cyanide baths were increased by the application of ultrasonics. Anode and cathode current efficiencies also were increased, and cell voltages were lowered; the relationship of these effects to current density is discussed. Electrode potential measurements showed significant depolarization effects at both electrodes during ultrasonic irradiation. The resulting decrease in cell voltage was due chiefly to depolarization at the anode, and the anode became less passive.

Jan 1, 1967

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 John Durkin

A computer model has been generated to evaluate speech intelligibility of individuals wearing conventional and electronic hearing protectors. For speakers talking at normal levels in noise levels of 65 db(Lp) or less, it was found that conventional hearing protectors significantly reduced speech intelligibility. Under the same conditions, electronic protectors provided scores equal to those for the unprotected individuals while providing protection from high noise levels. Therefore, electronic hearing protection is valuable in areas where high noise level is intermittent.

Jan 1, 1979

The extrapolation of results from reconstructed laboratory soil columns to field conditions is difficult because of the limitations of laboratory experiments. Permeability and elution tests performed in the laboratory differed from the natural state in that the soil was sieved through 1/4 inch screen to remove large stones and roots, its density was controlled by tamping the soil into two-inch I.D. tubes instead of normal weathering, and water and latex were applied with a constant head of liquid. Tube wall effects are important in interpreting data. Conversely, interpretation of field results were confounded by non-homogeneities within the sample tested, a soil profile with gradation of permeability and density with depth, and uncontrolled weather conditions and seasonal changes that affected the results. Nevertheless, both laboratory and field tests showed that a specific latex did perform as a soil sealant. In view of these facts a soil box experiment was designed to overcome some of the disadvantages associated with the small laboratory soil columns and the field experiments. Two wood soil boxes 5 ft x 5 ft x 5 ft were built in the greenhouse at the Uniroyal Research Center. They were lined with plastic PVC sheeting provided with tubes every six inches of depth on one side of each box to measure water removal rates under saturated conditions. Tensiometer gauges were placed at depths of 6, 12, 18, 24, 36 and 48 inches and Bouyoucos blocs and resistance thermometers were positioned at 6, 24 and 48 inch depths. Each box was filled with a uniform sub-soil obtained from Ogdensburg, N. J. The texture of this soil was determined to be a sandy loam by the ASTM Hydrometer method, as shown below: [ ] The boxes were thoroughly wetted by sprinkling to abet settling and allowed to dry by draining to check seepage ports and functioning of tensiometers.

Jan 1, 1972

By G. S. Rice

The Experimental Mine of the United States Bureau of Mines is a unique coal mine that serves as a large-scale testing laboratory. It is used primarily for testing the explosibility of coal-dust and gases but is also the workshop for many other kinds of research work of which the chief object is to increase safety in mining. The mine is situated in Allegheny County, Pa., about 13 miles southwest of Pittsburgh among the high hills of the west bank of the Monongahela River, at the northeastern edge of the gas-coal district of the Pittsburgh coal bed which extends south through the Connellsville coking-coal district into West Virginia. The Pittsburgh bed, of the Upper Carboniferous age, is one of the most extensive continuous coal beds in the United States, if not in the world. Throughout large areas it shows remarkable uniformity of thickness, levelness, and character of coal, which is a coking coal of high-grade bituminous rank. Its thickness in the northern part is 5 to 5 ½ feet and in the central and southern part is 7 to 9 feet.

Jan 1, 1933

By Marvin L. Whisman

Several parameters controlling the reproducibility of tritium determina¬tion in organic compounds by liquid scintillation counting were evaluated by the Federal Bureau of Mines. These included optimum volume of scintillator solution for maximum counting efficiency, reproducibility of counting a sealed commercial standard and comparison with duplicate counts on laboratory-prepared samples. The error introduced by using microliter pipets, optical differences in counting vials, reproducibility of counting organic samples where quenching is a factor, reproducibility of counting laboratory-prepared samples with an added internal standard, optimum ratio of internal standard activity to sample activity, effect of sample volume upon counting efficiency, count rate at which coincidence losses become apparent, and reproducibility of organic compound radioassay by the standard addition technique are outlined. From the evaluation of these parameters, a technique that can be applied routinely to organic compounds containing tritium has been established, and details are included in this report.

Jan 1, 1961

By H. E. Powell

Over 5 million lb of chromium, 1 million lb of nickel, and 90,000 lb of molybdenum are lost annually in the dusts generated in the production of stain-less steel. Additional losses of these metals in the form of mill scale and grinding swarf may be double the dust losses. This Bureau of Mines report describes a process for recovering these and other metals in the form of an alloy steel suitable for recycling. Zinc and lead, when present in the wastes, are recovered as byproducts in the form of oxide fumes. The laboratory-scale process (10-to 25-lb charges) recovers up to 95 pct of the chromium, 100 pct of the nickel, and 100 pct of the iron. The resultant alloy contains from 10 to 20 pct chromium, 6 to 12 pct nickel, and 55 to 65 pct iron, with lesser amounts of molybdenum and manganese. The alloy is essentially free of zinc, lead, and sulfur. The zinc-lead fume obtained from the treatment contains about 40 pct zinc and 20 pct lead and represents essentially complete recovery of these metals.

Jan 1, 1975

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 D. C. Dahlin

The U.S. Bureau of Mines investigated the magnetic susceptibility of minerals as a function of mag-netic field strength to determine how it might affect the potential for high-field magnetic separation as an alternative to other separation technologies. Single-mineral concentrates were prepared from specimens from the same deposit to compare magnetic susceptibilities of minerals that occur together and from specimens from different deposits to compare magnetic susceptibilities of like minerals. A vibrating-sample magnetometer with a superconducting magnet capable of producing a magnetic field of 7.16 x 106 Aim (90 kOe) was used to measure the magnetic moment of the samples. The data were then converted to specific magnetic susceptibility data and plotted as a function of magnetic field strength. Cursory studies were also completed on the effects of iron content and oxidation roasts on magnetic susceptibility in high fields. The results showed that magnetic susceptibility is essentially constant in magnetic fields above those needed to saturate ferromagnetic constituents. Although magnetic susceptibility is influenced by iron content and by thermal treatment, the changes are not large enough to influence separations in fields above 1.59 x 106 Aim (20 kOe).

Jan 1, 2010

By F. G. Horino

The Bureau of Mines conducted compressive strength tests on model pillars of selected rock types with each pillar containing a critically oriented plane of weakness. The objective of these tests was to determine if a significant increase in the strength of the model pillar could be obtained by either (1) installing tensioned rock bolts through the pillar and normal to the plane of weakness, or (2) wrapping tensioned steel wire ropes around the pillar at uniformly spaced intervals along the pillar. Equations based on Coulomb's failure criterion are developed to predict uniaxial compressive strength of model pillars that are either rock-bolted or wire-roped. Laboratory compressive strength tests on unbolted and bolted model pillars of sandstone, marble, Indiana limestone, and oil shale containing a plane of weakness oriented at 45° showed that the bolted pillars are stronger than the unbolted pillars by 84, 31, 52, and 28 pct, respectively. Laboratory compres-sive strength tests on nonroped and roped model pillars of Texas limestone, sandstone, and granite containing planes of weakness showed that the roped pillars were stronger than the nonroped pillars by factors ranging from 1.01 to 2.41, depending upon the angle of the plane of weakness and the rock type. Rocks with a low Young's modulus benefited most by the wire-roping technique.

Jan 1, 1971

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 Constantine C. Popoff

"INTRODUCTION AND SUMMARYDuring 1946 several high-grade limestone deposits in western Washington were examined by the Bureau of Mines. This report presents the data obtained from investigation of the Sauk Mountain deposits in east-central Skagit County, Washington.The investigation consisted of transit and topcgraphic surveys and sampling. The areas selected for sampling were first cleaned by blasting; channel samples up to 40 pounds were cut where practical. Chip samples averaging 30 pounds were taken where channel samples could not be cut. A total of 21 samples in the Sauk Mountain area were taken and. analysed. The locations of the samples are shown in figures 2 and 4, and the analyses are listed in tables 1 and 2. This investigation is a part of a long-range program of general investigation of mineral resources for future industrial development of the Pacific Northwest. The Sauk Mountain deposits were investigated for the purpose of disclosing now sources of high-purity limestone, which could be mined and shipped at low cost to Seattle and other industrial cities in the Pacific Northwest."

Oct 1, 1948

By F. Garacia, J. Cervik

Gob holes are routinely used by the mining industry to vent methane from gobs and to prevent it from entering the mine ventilation system. In some cases, flows from gob holes are measured by centering an anemometer on the end of a discharge pipe. These measurements are erroneous and tend to be high by as much as 30 pct. The Bureau of Mines deter- mined method factors (correction factors) for anemometer measurements taken in this manner. Method factors for 4-, 6-, and 8-in (10.2-, 15.2-, and 20.3-cm) ID pipe are 0.68, 0.71, and 0.78, respectively. Comparisons between horizontal and vertical flows indicated no significant change in method factors. Consequently, the method factors for horizontal pipe flows can be applied to vertical upward flows.

Jan 1, 1987