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By M. L. Whisman

Three samples of waste lubricating oil were re-refined by processes developed by the Bureau of Mines and reformulated with additives to meet designated requirements for viscosity and service. Quality-defining bench-scale tests were used to compare and evaluate the quality of these three motor oils, eight commercially re-refined lubricating oils, and three new lubricating oils. Most of the re-refined oils studied could not be distinguished from new oils by the bench tests used to define quality. There was some evidence, however, that one and perhaps more of the re-refined products investigated might not meet all of the quality standards of new lubricating oil, suggesting the need for better quality controls by re-refiners.

Jan 1, 1974

By C. Edward Chamberlain

A Bureau of Mines procedure was developed for the analysis of volatile matter in airborne coal dust-rock dust mixtures prior to, and resulting from, coal mine fires and explosions. Dust in the 10-to 20-mg weight range can be analyzed. Volatile matter is determined by a greatly scaled-down version of the empirical macro-scale method used by the Bureau. The alkaline earth carbonates in the rock dust are dissolved in acid prior to the volatile matter determination of the residue, and the rock dust content is calculated from the analysis of calcium and magnesium by atomic absorption.

Jan 1, 1974

By Henry E. Blake

The Bureau of Mines has been engaged in a continuing research effort to develop processes for increasing the recovery and utilization of fluorine from low-grade resources. This current research has shown that over 98 percent of the fluorine in phosphate rock is extracted when the ore is treated with excess phosphoric acid in the presence of water vapor at 150° to 180° C. More than 80 percent of the fluorine can be recovered as fluosilicic acid, which can then be converted to commercially useful hydrogen fluoride or fluorspar by previously developed Bureau processes. Extraction of P205 from the ore was about 98 percent in batch tests and 90 percent in semicyclic tests.

Jan 1, 1974

By F. P. Miknis

Previous studies at the Bureau of Mines have shown that broad-line nuclear magnetic resonance (NMR) techniques have potential applications for rapid evaluation of oil-shale deposits. In a continuation of this study the techniques of pulsed NMR have been applied in a similar manner. The basis for the pulsed NMR oil-shale assay method lies in the assumption that the free induction decay (FID) amplitude following a 90° pulse is proportional to the potential oil yield. This assumption was tested on two groups of oil-shale samples, numbering 141 and 263 samples, from two different oil-shale cores. For both groups of samples a small number were selected as calibration samples. Free induction decay amplitude measurements were made on the 141 and 263 samples. The best least-squares regression line was obtained for the calibration samples, and the oil yields of the remaining samples were calculated using the slopes and intercepts obtained in the regression analyses. The agreement between measured and calculated oil yields was good, the indexes of determination being 0.93 and 0.89 for the groups of 141 and 263 samples, respectively.

Jan 1, 1974

By Seth C. Schaefer

The Bureau of Mines studied thermodynamic properties of Al-Ni alloys con¬taining 0.54 to 30.04 atomic percent nickel with the aid of the high-temperature galvanic cell Al(1) // Al+3 (AlCl3 in NaCI.KC1) // Al-Ni alloy (1 or s). Activities of aluminum and nickel (compared with pure liquid metals as the standard state) show pronounced negative deviation from Raoult's law at 1,273 K. The properties [?G, ?Gxs, ?G ideal, ?GA1, AGxs1, ?Gni , and ?GNixs] have been derived from the experimental data and are summarized in tables and illustrations. At 1,127 K, the thermodynamic stability for the invariant three-phase equilibrium consisting of a saturated liquid, A13Ni, and A13Ni2 has been uniquely defined by an activity for aluminum of 0.751. A free energy of formation at 1,127 K of -7,940 cal/g-atom was derived for the compound A13Ni.

Jan 1, 1975

By R. L. Schmidt

Research conducted over the past 20 years in France, Great Britain, and the United States on the use of the large-hole burn cut has established cer¬tain advantages for this system. Advantages include longer pull and more complete fragmentation from blast rounds. However, research is needed to establish a set of parameters for optimum performance. As part of the Bureau of Mines Advancing Mining Technology for Marginal Resources program, the Twin Cities Mining Research Center, Twin Cities, Minn., acquired a horizontal rotary drill capable of boring holes up to 24 in. in diameter. This was used for a series of underground experiments at White Pine mine, White Pine, Mich., during 1973. Exceptional results were obtained with a 12-1/4-in void hole that yielded up to 18 ft of pull in a 10- by 20-ft drift, Fragmentation was excellent, and the compactness of the muck pile facilitated loading.

Jan 1, 1975

By J. B. Janus

This report continues a series of analyses of coal samples made by the Bureau of Mines in connection with the yearly purchase of several million tons of coal for various Government agencies. Listed are the analytical data on the composition and quality of tipple and de livered samples of coal collected during fiscal year 1974.

Jan 1, 1975

By Robert W. Freedman, Robert L. Craft, William G. Humphrey

As part of a continuing effort to reduce the weight and bulk of equipment that mining personnel must carry underground, the Bureau of Mines and the Mining Enforcement and Safety Administration (MESA) investigated accurate and convenient gas samplers for use by mine inspectors in sampling mine atmospheres. The samplers are septum-stoppered glass vials commonly used for routine blood sampling. These lightweight, compact samplers yield results comparable with those obtained with conventional bottle samplers of 250-ml nominal capacity.

Jan 1, 1975

By Robert W. Freedman

As part of a continuing effort to reduce the weight and bulk of equipment that mining personnel must carry underground, the Bureau of Mines and the Mining Enforcement and Safety Administration (MESA) investigated accurate and convenient gas samplers for use by mine inspectors in sampling mine atmospheres. The samplers are septum-stoppered glass vials commonly used for routine blood sampling. These lightweight, compact samplers yield results comparable with those obtained with conventional bottle samplers of 250-ml nominal capacity.

Jan 1, 1975

By D. H. Desy

The Bureau of Mines has conducted research on the ignition of methane-air mixtures by sparks caused by frictional impact of aluminum alloys on rusted steel at typical coal mine fan speeds. The objectives were to establish the incendivity of aluminum alloys under these conditions, to investigate differences between aluminum alloys, and to evaluate substitute materials for the aluminum-steel combination. With a specially designed apparatus, three commercial aluminum casting alloys and a number of experimental aluminum alloys were tested for incendivity of the frictional impact against rusted steel in flammable methane-air mixtures. All aluminum alloys tested produced some ignitions. Of the experimental alloys, the harder alloys and those containing silicon tended to be more incendive than the others. With the normal experimental conditions, constructional steel, stainless steel, brass, and plastic did not cause ignition of methane-air mixtures in frictional impact against rusted steel. Some ignitions occurred with constructional steel at high speed in more flammable gas mixtures enriched with oxygen. From these findings, it is suggested that constructional material combinations other than the aluminum-steel combustion would minimize this inc endive hazard. A detailed description is given of previous research, and comparison is made with present results where appropriate.

Jan 1, 1975

By F. P. Haver

Because State and Federal agencies have limited the amount of sulfur oxides that can be discharged to the atmosphere, most copper smelters plan to convert the S02 in offgases to sulfuric acid. In some cases, however, it might be preferable to use a nonsmelting method to fix the sulfur in the form of a discardable product. Research by the Federal Bureau of Mines has shown that sulfur in copper concentrate can be converted into insoluble anhydrite (CaS04) by roasting the concentrate with lime (CaO). After leaching the calcine to recover metal values, the residue may be discarded without harm to the environment. The process can use a rougher flotation product, thus reducing separation costs and saving valuable minerals (for example, molybdenite) that are now lost in making cleaner concentrate. In tests, rougher concentrate was pelletized with the theoretical amount of lime and roasted for 1 hour in a 6-1/2-inch-ID by 11-foot-long rotary kiln at 700° C. Sulfur retention was about 97 percent. Leaching the calcine with 20 percent RCI extracted approximately 99 percent of the copper, 73 percent of the iron, and 91 percent of the molybdenum. After the molybdenum was removed from the leach solution by adsorption on activated carbon, copper with a purity in excess of 99 percent was obtained by cementation on sponge iron. The strip solution then could be spray-roasted at 500° C to recover the RCI for recycle and obtain F2O3 as a byproduct.

Jan 1, 1975

By Lawrence K. Barker

Crude shale oil produced by underground retorting of Green River Formation oil shale was hydrogasified over a cobalt-molybdate-on-alumina catalyst at operating temperatures ranging from 800° to 1,300° F, pressures of 500, 1,000, and 1,500 psig, and a liquid hourly space velocity of 1.02 volumes of oil per volume of catalyst per hour (Vo/Vc/hr). At a temperature of 1,300° F and pressure of 1,500 psig, 94 weight-percent of the liquid feed was converted to gas containing 72 volume-percent methane. With two reactors in series at a temperature of 1,170° F in reactor 1 and 1,260° F in reactor 2 and a pressure of 1,500 psig, 97 weight-percent of the liquid feed was converted to gas with a methane content of 75 volume-percent. Liquefied petroleum gas (LPG) was hydrogasified at operating temperatures ranging from 500° to 1,400° F at a pressure of 500 psig over a cobalt-molybdate-on-alumina catalyst. Similar experiments were made with an empty tubular reactor. The data indicate that gasification reactions in the presence of a cobalt-molybdate catalyst change from predominantly a catalytic (carbonium ion) reaction to predominantly a thermal (free radical) reaction at temperatures greater than 1,100° F. The data also indicate that a reaction temperature of 1,350° F is necessary at the space velocities used in this investigation to make a synthetic natural gas (methane content of 90 volume-percent) from in situ crude shale oil.

Jan 1, 1975

By H. R. Appell

The Bureau of Mines studied the conversion of a variety of cellulosic wastes, for example, sawdust, bovine manure, sewage sludge, urban refuse (free of metal and ceramics), etc., to heavy oils. The objective of the investigation was to determine the scope of the reaction and elucidate the chemistry involved. The reactions took place in the presence of synthesis gas and water or carbon monoxide and water under conditions of elevated temperatures and pressures. Waste conversions above 90 pct, often near 99 pct, with oil yields in the range of 40 to 60 pct, were obtained in the temperature range of 250° to 425° C and pressure range of 1,500 to 4,000 psig. Because mild conditions were sought, most of the experiments were conducted at temperatures of 250° to 350° C and pressures of 1,500 to 3,000 psig. In general, lower viscosity products were obtained at higher reaction temperatures. Conversions and oil yields were significantly increased by operating in the presence of a high-boiling oil; either anthracene oil or oil recycled from the process was satisfactory. Synthesis gas containing 50 pct carbon monoxide gave satisfactory results as a replacement for carbon monoxide. Cobalt molybdate on alumina catalyst, used with sodium carbonate, gave a product of lower viscosity and lower oxygen content than sodium carbonate used as the sole catalyst. The waste-to-oil process has been successfully investigated in continuous flow equipment as well as in batch autoclaves.

Jan 1, 1975

By R. E. Siemens

A process is being developed by the Bureau of Mines to selectively recover nickel and cobalt from low-grade domestic laterites. In laboratory evaluation of the process, the oxides in the laterite were selectively reduced with carbon monoxide at temperatures from 350° to 600° C. For material containing more than about 5 percent magnesia, pyrite additions or post-reduction heat treatments were necessary to achieve satisfactory nickel and cobalt extraction for this range of reduction temperatures. Multistage leaching of the reduced material at ambient temperature and pressure in the presence of oxygen, ammonium sulfate, and ammonium hydroxide extracted up to about 90 and 85 percent of the contained nickel and cobalt, respectively. The nickel was selectively recovered from the leach solution by solvent extraction and was then stripped from the loaded organic with dilute sulfuric acid to provide a nickel-rich electrolyte. Treatment of the raffinate with hydrogen sulfide resulted in the recovery of cobalt as a sulfide. The only contaminant in solution was magnesium which was removed by ion exchange or precipitation. In this process the energy requirements are relatively low and except for minor operation losses, only coke and oxygen are consumed.

Jan 1, 1975

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 E. G. King

Enthalpy increments above 298 K were determined by the Bureau of Mines for magnesium hydroxide (brucite) between 298 and 900 K by the method of drop calorimetry. Enthalpy and entropy increments from this investigation were combined with other data from the literature to calculate absolute entropies, free energy functions, enthalpies of formation, Gibbs energies of formation, and equilibrium constants of formation from 298 to 900 K. By the use of published PVT data for water, a table of Gibbs energy change was given for the reaction MgO (periclase) + H2O = Mg(OH)2 (brucite) as a function of temperature and pressure.

Jan 1, 1975

By C. M. McCulloch

The methane content of virgin bituminous coalbed can now be measured accurately in the field with exploration core samples from vertical boreholes. The gas content of the coal per unit weight can be used either to design a mine ventilation system or to determine if degasification of the coalbed will be necessary before mining, and to determine the gas resources in the coalbed. The equipment necessary to conduct the test costs less than $50. The gas con-tent of the coal in place in the ground is determined by summing the gas lost from coring, gas measured during desorption, and the residual gas in the coal. Upon removal from the borehole, the core sample is placed in an airtight container and des orbed for several weeks until the desorption rate is below 0.05 cm3/g for 5 consecutive days. The gas lost from the core while it was being cored and the residual gas are estimated by a new graphical method. The amount of gas remaining depends upon whether the coal is friable or blocky. Friability appears to relate to the depth of the sample below the surface, fixed carbon percentage, Hardgrove grindability index, and proximity to tectonic disturbance. Friable coals emit nearly 96 pct of the total gas during desorption whereas a blocky coal emits only 60 pct of its total gas. Coalbeds that are ill defined as to their blocky or friable nature must be tested in the laboratory for unambiguous analysis.

Jan 1, 1975

By J. M. Stuve

Low-temperature heat capacities and the enthalpy of formation were deter-mined calorimetrically by the Bureau of Mines for CuO?CuS04. The derived standard entropy (S°298.15) was 40.36±0.04 cal/deg-mole, and the enthalpy of formation (?H°f) was -219.l±0.3 kcal/g-mole. A large thermal anomaly was observed in the heat capacity of CuO?CuS04 at 20±0.1 K. Gibbs energy of formation data are tabulated up to 1,200 K. Construction details of a precision low-temperature adiabatic calorimeter capable of determining heat capacities of solids in the temperature range 5 to 320 K are given. A calibrated miniature germanium resistance thermometer was incorporated into the calorimeter to extend the range of accurate measurements below 15 K. High-resistance dc heater windings were used throughout the cryostat to reduce heat conduction of inner connecting wires.

Jan 1, 1975

By W. S. Anderson

The use of flexible liners for support of underground openings has been investigated by the Bureau of Mines. This report presents installation procedures and instrumentation results of a full-scale flexible liner field installation in the Burgin mine. The flexible liner is a part of the mine support system and has provided maintenance-free support for 22 months

Jan 1, 1975

By D. G. Kuehn

Studies were conducted by the Bureau of Mines to determine the positive ions and neutral species produced in glow discharges of gas streams containing 1.0 percent NO in helium, 29 percent dry air in helium, and 1.06 percent NO in N2, Mass spectrographic measurements were conducted for gas pressures from 2.3 to 10.0 torr and dc currents from 10 to 20 mAo Ion species observed included NO+, N2 +, O2 +, N+, and 0+ with lesser amounts of He+, He2+, and N02+. Variations in various ionic and neutral species with discharge duration were interpreted to be consistent with an electrically induced dissociation of NO to produce N2 and O2. No nitrogen oxides were observed to form in glow discharges of the helium-air mixture.

Jan 1, 1975