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The National Personal Protective Technology Laboratory (NPPTL) of the National Institute for Occupational Safety and Health (NIOSH) has undertaken a collaborative study with the Mine Safety and Health Administration (MSHA) to determine how well self-contained self-rescuers (SCSRs), deployed in accordance with Federal regulations (30 CFR 75.1714), withstand the underground coal mining environment with regard to both physical damage and aging. Apparatus tested included the CSE SR-100, the Draeger OXY-K Plus, the MSA Life-Saver 60, and the Ocenco EBA 6.5 and M-20. This report presents findings regarding laboratory-tested SCSRs in the tenth phase of testing, from July 2004 to March 2006. The SCSRs were tested on a breathing and metabolic simulator and on a human subject walking on a treadmill. The tests performed in this study are not the tests used for certification (Title 42 of the Code of Federal Regulations, Part 84). The tests performed in this study continue until the apparatus are empty to enable comparison of new versus deployed apparatus. The method for obtaining deployed SCSRs for this evaluation was not a random selection from the deployed population of SCSRs. We sought older apparatus with visible environmental impact rather than newer apparatus, and we attempted to sample a wide range of deployment modes. Although the results of these tests are useful for observing performance of the tested SCSRs, they are not representative of all deployed SCSRs. This report is the last of 10 report phases begun in 1982. Previous reports describe phases 1 through 9 [Kyriazi et al. 1986; Kyriazi and Shubilla 1992, 1994, 1996, 2000, 2002, 2004, 2006] A new evaluation protocol, with revised sampling strategies, test methods, and reporting procedures, is currently being designed to enhance the applicability of the results. The results of these studies suggest that the large majority of SCSRs that pass their inspection criteria can be relied upon to provide a safe level of life support for mine escape purposes. However, the storage and handling in the mining environment seems to have caused performance degradation in some of the apparatus. In this phase, phase 10, we found some CSE SR-100s (93 tested) that exhibited high CO2 levels, stuck-together breathing hoses, starter-O2 failure, breathing hose punctures and tears, high breathing pressures, and loose particulates in the breathing hose. The loose particulates caused coughing in human-subject tests. One MSA Life-Saver 60 (20 tested) in this phase had a stuck-open relief valve. One Ocenco EBA 6.5 (50 tested) had an unattached O2 supply hose. An unexplained phenomenon occurred with two Ocenco M-20s (20 tested): low O2 flow rates preventing their successful use. Almost all of the failures noted involved units that failed their inspection criteria.

Jan 6, 2008

By R. P. Beyer

Low-temperature heat capacities and standard enthalpy of formation of copper difluoride (CuF2) were determined by the Bureau of Mines. The low-temperature heat capacities were determined from 11 to 302 K by adiabatic calorimetry. The enthalpy of formation was determined by HC1 solution calorimetry. The standard values of entropy (S°) and enthalpy of formation (?Hf°) at 298.15 K are l8.65±0.03 cal/deg mole and -129.02±0.29 kcal/mole, respectively.

Jan 1, 1978

By J. M. Stuve

The standard heats of formation (?Hf°) of holmium trichloride and terbium trichloride were measured by solution calorimetry. Heats of solution of holmium and terbium metals and their anhydrous chlorides were measured in 4.360 molal HCI at 298.15° K. From these measurements ?Hf° for HoC13 (c) was calculated as -240,290 ±1,700 cal/mo1e, and ?Hf° for TbC13 (c) was calculated as -238,330 ±1,500 cal/mole at 298.15° K.

Jan 1, 1967

By R. Barany

The heats of formation of anhydrous ferric sulfate and anhydrous indium sulfate were determined by solution calorimetry. At 298.15° K the heats of formation from the metal, rhombic sulfur, and oxygen were -615.6 ±O.7 kcal/mole for ferric sulfate and -649.6 ±O.6 kcal/mole for indium sulfate. Heats of decomposition at 298.15° K are given for the reaction that forms metal oxide, sulfur dioxide, and oxygen) and for the reaction that forms the metal oxide and sulfur trioxide.

Jan 1, 1965

By W. W. Weller

Heat capacity measurements of anhydrous cobalt sulfate (CoSO4), copper sulfate (CuSO4), nickel sulfate (NiSO4), and zinc sulfate (ZnSO4) were conducted over the temperature range 51° to 298° K. The results were used to evaluate the following entropies at 298.15° K (cal/deg mole): CoSO4, 28.1; CuSO4, 26.8; NiSO4, 24.8; and ZnSO4, 26.4. Entropies were combined with heats of formation to give free energies of formation.

Jan 1, 1965

By R. Barany

The heats of formation of seven substances were determined by solution calorimetry. At 298.15° K, the heat of formation of lithium sulfate from lithium, rhombic sulfur, and oxygen was -343.1 ± 0.7 kcal/mole, and the heat of formation of lithium sulfate monohydrate from lithium, rhombic sulfur, oxy-gen, and hydrogen was -414.3 ± 0.7 kcal/mo1e. For the silicates, the heats of formation at 298.15° K from the elements were kaliophilite, -503.8 ± 0.5 kcal/mole; leucite, -721.6 ± 0,8 kcal/mole; eucryptite, -505,2 ± 0.6 kcal/mole; alpha-spodumene, -727.9 ± 0.9 kcal/mole; and beta-spodumene, -721.1 ± 0.9 kcal/mole. The corresponding heats of formation at 298.15° K from the constituent oxides were kaliophilite, -42.7 ± 1.1 kca1/mole; leucite, -42.8 ± 1.1 kcal/mole; eucryptite, -16.1 ± 0.7 kcal/mole; alpha-spodumene, -21.0 ± 0.7 kcal/mo1e; and beta-spodumene, -14.3 ± 0.7 kcal/mo1e.

Jan 1, 1966

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 J. M. Stuve

Calorimetric determinations of the low-temperature heat capacities, standard enthalpy of formation, and high-temperature enthalpies were made of (Na20)4 ?Fe20,(c). The resulting values of entropy (S°), enthalpy of formation (?Hf°), and free energy of formation (?Gf°) at 298.15° K are 104.676 cal/deg mole, -656.2 ±.kcal/mole, and -603.4 A kcal/mole, respectively. Tabulations of Cp°, S°, - (G°-H°298)/T, H°-H°298, ?Hf°, ?Gf°, and log Kf are given to 1,200° K.

Jan 1, 1971

By William J. Campbell

The possibility of chemical analysis by identification of characteristic X-ray spectral lines was first suggested by H. C. J. Moseley in 1913.3/ For a given spectral series it was found that the frequency of the characteristic radiation was proportional to the square of the atomic number of the excited atom. Siegbahn and his coworkers improved the instrumentation and accurately determined the wavelengths of the characteristic spectra for most of the elements .4/ In fluorescent X-ray spectroscopy, the characteristic X-rays of atoms are emitted or fluoresced upon absorption of primary or incident X-rays of shorter wave-lengths (higher energies). The K spectral lines are used for elements of atomic numbers 13 to about 63, and the L series for those above atomic number 50. Whether the K or L lines are used for elements 50-63 depends upon the type of instrumentation available. The laboratory at the Eastern Experiment Station of the Bureau of Mines, College Park, Md., uses the K lines up to atomic number 57 and the L lines for thong elements of higher atomic number.

Jan 1, 1955

By James R. Welty

Heat content values were experimentally determined for yttrium metal between temperatures of 400° and 1,300° K and for iron pentacarbonyl between 301° and 380° K. The drop technique was used; that is, a sample of material sealed in a protective capsule was heated to 3 desired temperature in a furnace and then dropped into an ice calorimeter. A revised technique for determining heat content values from calorimetric data is described. Heat content and corresponding entropy-increment data above a reference temperature of 298.15° K are presented in tabular form. Equations for heat content and heat capacity as functions of temperature were derived for each substance. These equations are [Y (c): HT-H298.15 = 1.2041T 1 3.393 x 10-3T2- 0.4176 x 10' T"1 + 739.9 cal/mole Cp = 1.2041 + 6.786 x 10-3T + 0.4176 x 106-T-2 cal/deg mole Fe (CO) E, (1) : HT - H298.15 = 55.636T - 16,588 cal/mole Cp = 55.636 cal/deg mole]

Jan 1, 1963

By R. Barany

The heats of the glass-crystal transformation of nepheline (Na0.7794K0.2206AlSiO4) and wollastonite (CaSiO3) and the heat of formation of nepheline at 298.15° K were determined by solution calorimetry. For the glass-crystal transformations, the heat values were -9.0 ± 0.3 kcal/mole for nepheline and -8.1 ± 0.2 kcal/mole for wollastonite. The heat of formation of nepheline was -34.8 ± 0.6 kcal/mole from the oxides and -501.0 ± 0.5 kcal/mole from the elements.

Jan 1, 1966

By W. W. Weller

Low-temperature heat capacities of scandium sesquioxide (Sc203) and a mixture of cerium sesquioxide (Ce203) and cerium dioxide (CeO2) were measured over the temperature range from 50° to 298° K. The entropy of scandium sesquioxide at 298.15° K was evaluated directly as S°298.15 = 18.4 ± 0.1 cal/deg mole. That of cerium sesquioxide was extracted by combining the heat-capacity data for the mixture with those for pure cerium dioxide; the result was S298.15 36.0 ± 1.0 cal/deg mole.

Jan 1, 1963

By Stephen D. Hill

The Bureau of Mines devised and constructed a modified Knudsen effusion apparatus, permitting a constant measure of the weight of effusing vapor, to determine the equilibrium vapor pressure of metal halides at temperatures up to 1,200° K and over the pressure range 10-5 to 10-2 torr. The reliability of the apparatus was established by determining the vapor pressure of potassium chloride. After correcting for partial dimerization of the vapor, data obtained on solid KCl between 750° and 950° K can be expressed by the following equation:

Jan 1, 1966

By E. A. Loria

The Bureau of Mines analyzed the effects of oxygen, nitrogen, and carbon on the tensile properties of electrorefined vanadium in terms of the Petch equation. The effects of the different impurities and grain sizes on the yield and flow stress between 2730 and 770 K were studied. For specimens of like composition, the values of the Petch parameters 01 and ky obtained by two different methods, extrapolation and grain size, were nearly the same. For high-purity electrorefined vanadium, the 01 value at 2730 K was 10,300 psi (5,150 psi shear). The 01 values for this metal at 1950 and 2730 K were lower by factors of 3 to 4 than for three less pure samples of commercial vanadium metal of equivalent grain size. Nitrogen was more effective than oxygen in increasing 01' the increase being about twice as much for the same impurity level. Carbon produced a slight increase in 01 up to 0.024 percent and then a gradual decrease in 01 to 0.11 percent, the maximum carbon content studied. The corresponding ky values followed the same trend in regard to oxygen and nitrogen additions, whereas the addition of carbon produced no variations at either temperature. Dislocations in vanadium are anchored by carbon, oxygen, and nitrogen with increasing firmness in that order. The high purity of electrorefined vanadium was confirmed by low yield stress and high ductility throughout the low temperature range. The metal also exhibited profuse twinning with high ductility at 1230 and 770 K. The effective surface energy for fracture, y, was found to lie between 3.3 and 3.6 x 1()4 erg cm-2?

Jan 1, 1966

By Michael J. Sapko, Eric S. Weiss, Kenneth L. Cashdollar

A fundamental safety research area for the National Institute for Occupational Safety and Health (NIOSH) is to eliminate the occurrence of coal mine explosions or to mitigate their effects. One approach is to develop and evaluate new and innovative seal designs that provide increased explosion protection for mining personnel. The NIOSH Pittsburgh Research Laboratory (PRL) cooperated with HeiTech Corp. of Virginia, Barclay Mowlem Construction Ltd. of Queensland, Australia, and the Mine Safety and Health Administration (MSHA) in three separate research programs to evaluate the strength characteristics and air leakage resistance of numerous innovative seal designs and ventilation control structures for use in underground coal mines. For each phase of the program, various full-scale seals, stoppings, and an overcast design were constructed in PRL's Lake Lynn Experimental Mine near Fairchance, Fayette County, PA. The seals and stoppings were built in crosscuts and were subjected to explosions to evaluate their strengths. Four pumpable cementitious seal designs ranging in thickness from 610 to 915 mm (24 to 36 in) were evaluated in the first cost-reimbursable research program with HeiTech Corp. A simple wooden framework with brattice liner was used as a form to contain the cementitious slurry during the curing period. As the seal designs decreased in thickness, higher compressive strength cementitious grout was used. All four seals withstood an explosion pressure pulse of at least 138 kPa (20 psi) while maintaining acceptable air leakage resistance. In the second cost-reimbursable research program with Barclay Mowlem Construction Ltd. of Australia, several innovative seal and stopping designs and an overcast design were evaluated. Each of the seal designs and the overcast side and wing walls used one or more air-inflated vinyl bladder assemblies anchored to the mine roof and hitched into the ribs and floor. The air within these bladders was displaced with a high-strength cementitious grout. The overcast deck consisted of a 200-mm ('7.8-in) thick reinforced cementitious slab. This was the first time that an overcast structure had been explosion tested under full-scale conditions. All of the seals, stoppings, and overcast design passed the air leakage tests before being subjected to a series of explosions with static pressure pulses ranging from 14 to 475 kPa (2 tab 69 psi). Instrumentation measured seal and overcast wall displacement as a function of time. The 450-mm (1 7.7-in) thick seal in the 2.8-m(9-ft) high third crosscut withstood an explosion pressure of 170 kPa (25 psi), but failed during a later test, which generated a peak static pressure of 475 kPa (69 psi) at the seal location. A similar 450-mm-thick seal in the 2.1-m (7-ft) high second crosscut withstood three explosion tests, which generated peak static pressures of 195, 205, and 370 kPa (28, 30, and 54 psi) at the seal location. Next, the overcast design withstood four explosions, which generated static overpressures ranging from 16 to 47 kPa (2.3 to 6.8 psi). A third program at the request of MSHA evaluated the effectiveness of using pressurized grout bags (Packsetter bags) along the mine roof and ribs in lieu of floor and rib hitching for a standard-type solid- concrete-block seal. This program was initiated to address an urlusual geological mining condition encountered when building seals in entries where required rib hitching is not a viable option due to soft friable coal. Results showed that the use of these quick-setting grout-filled Packsetter bags pressurized internally to 300 kPa (44 psi) not only provides a seal that can withstand a 138-kPa static pressure explosion, but also provides a sealing option where rib hitching is not possible.

Jan 1, 2003

By K. O. Bennington

[Thermodynamic properties of two amphibole asbestos minerals were determined by the Bureau of Mines. The enthalpies of formation were determined by the hydrofluoric acid solution calorimetry method. Heat capacity measurements were made with an adiabatic calorimeter over the range of 5 to 315 K. High-temperature enthalpies above 298 K were determined with a copper-block drop calorimeter to 852 K for amosite and to 902 K for crocidolite. Thermodynamic data determined for amosite of the composition Fe5+2.2766Mg1.5209 Fe+03.12Mn0.0825) Si7.9163Al0.0837022.0363)(OH)1.9637 are: S°298 = 168.8 ± 5 cal/deg-mole; ?Hf°298-15 (elements) = -2419.24 ± 2.95 kcal/mole; ?Hf298.15 (oxides) = -30.92 ± 2.47 kcal/mole; and ?Gf° -2260.1 kcal. Corresponding data found for s3 ,1s = crocidolite of the composition (Na1.9Ca0.1)(Fe2+.024Fe2.5 01Mg0.475) (Si7.9713024Fe+2 2.501Mg0.475) (Si7.971 Al0.029022.095) (OH)1.905 are: S2.98-15 - 161.1 ± 4 cal/deg-mole; ?Rf° 2 298.15 (elements) = -2433.56 ± 2.99 kcal/mole, 10298.1s (oxides) = -87.69 1.70 kcal/mole, and ?Gf°298.15 = -2269.8 kcal.] Calorimetric values from this investigation were combined with other data from the literature to calculate the Gibbs energies of formation and equilibrium constants of formation over the temperature range of the measurements. Tables of enthalpies of formation and Gibbs energies of formation are given as a function of temperature both from the elements and the constituent oxides.

Jan 1, 1978

By Mark Davis

As a follow-on to previous investigations, reduced treatment levels for the optimum fire retardant/preservative system were evaluated. An impregnation of 3.5 lbs/ft3 of Fyreprufe followed by 3.5 mils of Albi 107A plus an Albi 144 top coat provides adequate flammability and flame spread protection. However, there is a significant loss in compressive strength at this retention level, particularly parallel to the grain. A pilot-size pressure impregnation cell was installed for use in treating larger quantities of wood. Based on the optimum fire retardant/preservative treatment system - Fyreprufe/ACC impregnation followed by Albi 107A/144 intumescent paint - a model treatment pro¬cess was developed, capable of handling 3 million board feet per year. Associated annualized costs per thousand board feet (K bd. ft.) for treating 12" x 12" timber were calculated to be: Impregnation: $-63.00/K bd. ft. Coating: $112.00/K bd. ft. A literature search was conducted to identify materials and techniques suitable for a localized stench warning system for heated mine timbers. Based on this review, a number of stench warning concepts were developed. Those based on surface coating were given a preliminary laboratory evaluation.

Jan 1, 1982

By Philip Thompson

A part of the Bureau of Mines mission is to help improve the Nation's mineral posture by providing the technology for utilizing low-grade ores. In this regard, laboratory testing by the Bureau of Mines has shown that the removal of insoluble slimes using selective flocculation and flotation is a viable method for treating low-grade potash ores that have a high content of water-insoluble impurities. Results indicated that over 82 percent of the insoluble slimes could be removed from sylvinite ore containing 5 percent water insolubles and 13 percent K20 by using nonionic or cationic polyacrylamide flocculants and cationic, anionic, and/or nonionic collectors. Subsequent potash flotation recovered 87 percent of the potash in rougher concentrates containing 57 percent K2O. Sizing and cleaner flotation of the rougher concentrates upgraded the products to 60 percent K2O. Filtration of the water-leached insoluble-slimes flotation concentrates on a bed consisting of leached insoluble-slimes concentrate mixed with potash flotation tailings recovered 80 percent of the brine. Filtration rates using the mixed bed were nine times faster than filtration rates obtained when the insoluble-slimes flotation concentrates were filtered separately.

Jan 1, 1979

By J. I. Paige

As part of a continuing effort to develop technology that maximizes mineral and metal recovery from domestic resources, the Bureau of Mines investigated a method to totally utilize copper converter slags without recycling them back through the matte smelting furnace. The research was directed toward (1) recovering the contained copper in converting slags by producing a recyclable copper-iron matte, (2) carbothermically reducing the slags to recover the iron, and (3) producing slag wool from the depleted slags. This report deals with the reduction of three industrial converting slags, containing 2.0 to 7.3 wt-pct Cu, in an 800-kVA electric arc furnace to produce a recyclable copper-iron matte. The addition of sufficient iron pyrite to provide 29 to 113 pct of the stoichiometric sulfur (based on producing 40-pct-Cu matte) produced a recyclable matte (36 to 61 pct Cu) at an energy consumption of 520 to 700 kWh per ton of solid material charged. The expected energy saving for treating molten slag in an electric furnace (5-to 9-MVA range) is about 400 kWh per ton of molten slag treated.

Jan 1, 1982

By E. G. King

Low-temperature heat capacity determinations of the minerals goethite and pyrophyllite were made in the temperature range from 510 to 298° K. The entropies at 298.15° K were evaluated as 14.43 ±0.15 cal/deg mole for goethite and 56.6 ±0.5 cal/deg mole for pyrophyllite. The entropies of formation from the constituent oxides are -4.4 ±0.2 cal/deg mole for goethite and -12.3 ±0.6 cal/deg mole for pyrophyllite. The standard free energy of formation of goethite from its oxides is ?G°298.15 = 0.16 ±0.20 kcal/mole.

Jan 1, 1970