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By E. G. Davis

Large-scale ultrafine grinding tests of a coarse kaolin were made using the Bureau of Mines developed attrition grinding process in continuous open-and closed-circuit systems. A 20-inch diameter attrition grinder, designed and constructed at the Tuscaloosa Laboratory, was used. Studies included single- and multiple-stage open-circuit grinding, and also continuous grinding tests in closed-circuit with a 6-inch-diameter solid bowl centrifuge. Clay feed, containing 9.0 percent minus-2-micrometer esd, was used at fates up to 840 pounds per hour. Multistage grinding tests gave better results than single-stage treatment when equivalent clay feed rates were used. Closed-circuit grinding tests yielded ground products containing slightly more minus-2-micrometer-esd clay than the open-circuit grinding when using the same clay feed. Energy consumption was lower in closed-circuit grinding than in batch or open-circuit grinding. A modified two-stage closed-circuit grinding system gave the best grade of product and amount of minus -2-micrometer-esd clay produced per pound of clay feed. The ground product from this test contained 88.5 percent minus-2-micrometer-esd material and electrical energy consumption was 327 kilowatt-hours per ton of minus-2-micrometer-esd material produced.

Jan 1, 1973

By William J. Campbell

This analytical method development and evaluation was undertaken by the Bureau of Mines to provide accurate determinations of eight minor elements in low-alloy steels prepared from ferrous scrap. Fluorescent X-ray spectrography was the principal method investigated. Confirming analyses were made by conventional instrumental and chemical methods. All X-ray data were processed by a timesharing computer. No corrections were found necessary for inter-element effects or overlapping spectral lines. Concentrations were calculated from the least-square fit of a linear calibration equation derived from measurements on three sets of standard steels. These studies show that X-ray spectrographic analysis of lathe-finished surfaces provides accurate determinations of aluminum, copper, chromium, manganese, nickel, phosphorus, silicon, and tin.

Jan 1, 1973

By J. B. Rosenbaum

Prolonged laboratory and limited pilot plant tests have shown that the Bureau of Mines buffered S02 -H2S process is capable of removing 95 to 99 percent of the S02 from industrial waste gases. Most of the S02 is converted to elemental sulfur; only about I percent converted to sulfate The process comprises (1) washing the flue gas to remove particulates and S03, (2) absorption of the S02 in citric acid or other carboxylate solution, (3) reaction of the loaded solution with H2S in a closed vessel to precipitate the absorbed S02 as elemental sulfur, and (4) separation of the sulfur from the regenerated solution by oil flotation and melting. Two-thirds of the molten sulfur is converted to H2S for use in the sulfur precipitation step by reacting sulfur vapor with natural gas and steam in the presence of an alumina catalyst. The chemistry and mechanism of the process are described, initial laboratory and pilot plant data are summarized, and second-generation laboratory operation and pilot plant design are reviewed. Preliminary cost estimates are presented for recovering sulfur from copper smelter gas, powerplant flue gas, and Claus plant tail gas.

Jan 1, 1973

By L. L. Oden

The purpose of this research was to develop a method to remove copper and tin from the magnetic fraction of incinerated municipal refuse, as recovered by the Bureau of Mines pilot plant in College Park, Md. Copper, present in the scrap in a metallic form bonded to ferrous objects, was amenable to leaching in cupric ammonium carbonate solution. Copper levels in small 5-to 10-lb lots of treated scrap were reduced from the initial level, 0.5 to 0.6 pct, to 0.1 to 0.2 pct. Larger lots of scrap (100 lb) were treated less effectively because of poor contact of solution and scrap. Oxidation in the air or in aerated aqueous solution was applied to liberate tin from the dilute solid solution present on the surface of incinerated tinplate. Shredding of air-oxidized scrap or caustic leaching of scrap oxidized in solution reduced tin levels from the initial 0.25-pct level to about 0.1 pct.

Jan 1, 1973

By L. A. Haas

Hydrogen sulfide was decomposed to elemental sulfur in an electrical discharge. With He, N., or Ar diluents, a threshold voltage between 1 and 3 kV was required for the decomposition reaction to occur in a laboratory ozonizer. Above the threshold voltage, the HAS decomposition rate increased with increasing voltage, but the increase was more pronounced with argon diluent than with either nitrogen or helium. In common with other reactions in an electrical discharge, the B2S decomposition decreased with increasing temperature in the range of -410 to +61° C. The reaction did not appear to be rate-controlled by a solid-gas sorption step because the introduction of activated charcoal into the electrical discharge zone did not significantly affect the decomposition yield. In the presence of polymeric chlorofluoro-carbon oil, 90 pct conversion of the 3 pct H2S in helium was obtained at 14 kV, 60 Hz, a 2-mm electrode gap, and a gas-residence time greater than 1 min. Under the same experimental conditions in the absence of oil, the conversion was only about 50 pct.

Jan 1, 1973

By Charles W. Huggins

To determine the nahcolite and dawsonite content in oil shales, the Bureau of Mines compared X-ray diffraction, infrared spectroscopy, thermal methods, and a previously published method by Smith and Young based on the selective solubility of sodium compounds. The Smith and Young method and a new method based on the weight of carbon dioxide produced by thermal decomposition are recommended for determining nahcolite. X-ray diffraction and the Smith and Young method are recommended for determining dawsonite. X-ray diffraction, infrared spectroscopy, and differential thermal analysis were useful for identifying other minerals in the samples.

Jan 1, 1973

By Joseph Grumer

In addition to nine powder and gaseous extinguishants of propagating Pittsburgh seam coal dust-air explosions earlier evaluated,6 10 other powders have similarly been evaluated under like conditions such that wall quenching of the coal dust-air flames was virtually absent and the dust concentration was temporally and spatially uniform to within about ±5 percent. None of the newly examined extinguishants was better than Purple-K (potassium bicarbonate); the 10 of this report are anhydrite (calcium sulfate), monobasic (4 types) and dibasic ammonium phosphate, natural and synthetic cryolite (sodium fluoalumi-nate), sodium sulfate, and tricalcium phosphate. Except for anhydrite, sodium sulfate, tricalcium phosphate, and the cryolites, these materials were about equally effective, when present in relatively low concentrations (weight-percent of the coal dust-extinguishant mixture). The maximum oxygen concentration for the extinguishment of otherwise uninhibited coal dust explosions and the influence of coal dust particle size and the volatile content of the coal were also explored. For the present, the choice of the inhibitor among the good ones evaluated is not as critical as the system to be used to deploy the extinguishant against a coal dust explosion.

Jan 1, 1973

By F. E. Spencer

This Bureau of Mines report provides a complete mathematical description of the algorithm employed by a general multiphase chemical equilibrium program developed particularly for the purpose of studying problems in coal combustion, although the generality of the program will allow its application to any equilibrium system in which an appreciable gas phase is present. When applied to coal combustion problems, the program predicts composition and quantity of slag and unconsumed carbon phases as well as calculates accurately the composition of the gas phase including trace species such as free electrons and ions which are important for predicting electrical properties.

Jan 1, 1973

By Parviz F. Rad

The increased use of tunnel boring machines (TBM) has stimulated laboratory research to optimize the cutting parameters of these machines with the objective of increasing machine efficiency and penetration rate. Laboratory-scale rock cutting experiments have succeeded in identifying many of the important parameters involved in rock-cutter interaction. Although scaling factors may be required to apply the results directly, the concepts developed can be used qualitatively as design guidelines for boring machines. The Bureau of Mines Twin Cities Mining Research Center has recently developed a large-scale rock cutting device (RCD) that will simulate many of the operating parameters of the tunnel boring machines in the laboratory under a controlled environment. The results of the experiments with this device will be directly applicable to the design of TBM's.

Jan 1, 1973

By Robert I. Fujimoto

The work described was conducted to develop standards for the application of wire rope clips on wire rope. These standards include optimum number of clips and clip nut torques for wire rope sizes 1/4 through 2-1/4 inches, when used for forming an eye attachment in wire rope. Wire rope test specimens with clip attachments were load tested on tensile testing machines to determine an effective combination of clip nut torques and number of clips for each size of wire rope to develop efficiencies above 90 percent of the catalog ultimate rope strength.

Jan 1, 1973

By Charles Findlay, Stephen Krickovic, J. E. Carpetta

As one of its projects for degasification of major panels of coal prior to mining within them, the Bureau of Mines conducted methane emission studies during development of a set of three headings 1,800 feet in a major coal panel (2,700 by 3,500 feet) which had been completely isolated by sets of main headings for 12 months in the Federal No. 2 mine (Pittsburgh coalbed) in northern West Virginia. Similar emission studies were conducted in the development of two sets of main headings in virgin coal areas nearby. Comparing the two sets of data indicated that the isolated coal panel had been degasified by approximately 70 percent.

Jan 1, 1973

By Rees D. Groves

The Bureau of Mines conducted research on reactions of copper sulfide minerals with chlorine in an aqueous system. Selected samples of covellite, chalcopyrite, chalcocite, bornite, and pyrite were leached with aqueous chlorine solutions. The mineral samples were sized on to minus 100- plus 325-mesh, individually mixed with precleaned sand and leached in an enclosed percolation column. Each mineral was leached in stages to achieve about 90 percent mineral dissolution. The chlorine leaching solutions were produced by reacting sodium hypochlorite with hydrochloric acid within the closed system. The study showed that when the mineral dissolution was complete, the reaction products (copper, iron, and sulfur) were in their highest oxidation states and a stoichiometric amount of chlorine was consumed. Although elemental sulfur formed as an intermediate product, it was oxidized to sulfate during the leach.

Jan 1, 1973

By R. E. Lindstrom

Electrooxidation techniques were investigated on a bench scale by the Bureau of Mines to determine the applicability of the process for extracting molybdenum and rhenium from low-grade molybdenite concentrates. Parameters affecting the extraction, such as pulp density, power consumption, reagent requirements for pH control, and electrolytic cell configuration, were studied. Molybdenum and rhenium extractions of 98 to 99 percent were achieved from several concentrates containing 4.76 to 28.6 percent molybdenum and 180 ppm to 1,000 ppm rhenium. Optimum results were obtained by maintaining pH values between 5.5 and 7.0 during electrolysis and allowing the final pH to rise to about 8.2. Reagent consumption was 4 to 6 pounds of sodium carbonate per pound of molybdenum extracted. The power consumption declined from a range of 12 to 25 kilowatt hours per pound of molybdenum extracted with immersion electrodes to 9.7 kilowatt hours with a bipolar flow-through cell; however, molybdenum extraction was independent of cell configuration.

Jan 1, 1973

By Stephen Krickovic, J. E. Carpetta, T. D. Moore

Air quantity-pressure and methane concentration surveys were conducted by the Bureau of Mines in accessible portions of an area being pillared in a Pittsburgh coalbed mine in West Virginia. These included two mined-out and three active butt headings and a bleeder system. The particular mine workings were started in virgin coal directly from a set of main headings; the main reason for the study was the difficulty usually encountered in adequately bleeding the gobs under such conditions. Although the two separate return airways in each active butt heading and the North and 1 Left bleeders contained acceptable methane concentrations (0.01 to 0.78 percent in the butts and 0.73 to 1.0 percent in the bleeders) with significant total methane removal (109 cfm in butts and 631 cfm in bleeders), there were relatively large areas in the gobs with possible minimal airflows. This condition appears to have developed from lack of systematic regulation of the airflow across the gobs and appears to indicate the existence of considerably more methane in the probably low flow areas in the gob.

Jan 1, 1973

By Stephen Krickovic

Air quantity-pressure and methane concentration surveys were conducted by the Bureau of Mines in accessible portions of an area being pillared in a Pittsburgh coalbed mine in West Virginia. These included two mined-out and three active butt headings and a bleeder system. The particular mine workings were started in virgin coal directly from a set of main headings; the main reason for the study was the difficulty usually encountered in adequately bleeding the gobs under such conditions. Although the two separate return airways in each active butt heading and the North and 1 Left bleeders contained acceptable methane concentrations (0.01 to 0.78 percent in the butts and 0.73 to 1.0 percent in the bleeders) with significant total methane removal (109 cfm in butts and 631 cfm in bleeders), there were relatively large areas in the gobs with possible minimal airflows. This condition appears to have developed from lack of systematic regulation of the airflow across the gobs and appears to indicate the existence of considerably more methane in the probably low flow areas in the gob.

Jan 1, 1973

A study was conducted by the Bureau of Mines to evaluate natural gas as an automotive fuel and to provide guidelines for optimum engine adjustments for low exhaust emissions. The study was conducted using a single-cylinder engine, a multicylinder engine, and a total of eight vehicles. Results from single-cylinder engine tests showed that the light-load, lean-limit misfire region for natural gas begins at an air-fuel ratio between 150 and 160 pct of stoichiometric. Changes in ignition timing significantly influenced emissions of nitrogen oxides and hydrocarbons, but had little effect on carbon monoxide emission. Low emissions can be achieved with current-design engines by adjustment of engine parameters, but only with heavy penalty to engine performance. Emissions from vehicles fueled with natural gas are virtually unaffected by ambient temperature change within the range 20° to 100° F. The organic emissions from engines fueled with natural gas were estimated to be 22 to 25 pct as reactive as the emissions produced using gasoline. Levels of exhaust emissions from vehicles fueled with natural gas were unchanged over 10,000 miles of normal driving.

Jan 1, 1973

By A. W. Hall

A nuclear method was developed for continuously and automatically deter-mining the moisture content of coal flowing through a bin. Fast neutrons from a 1 curie americium-beryllium source penetrate the coal, are thermalized (slowed down) by hydrogen in the moisture, and are counted by a thermal neutron detector. The difference between the number of these thermal neutrons and those thermalized by dry coal (in a reference drum) is a measure of the moisture content of the coal. A materials handling system was developed and in tests at a commercial coal preparation plant, moisture in coal was monitored continuously within 0.2 percent of values determined by conventional means. The meter responded rapidly to change in moisture content, making it adaptable to automatic process control, and was operated for 1 year without malfunction or recalibration. Shielding of the source by the coal kept the neutron flux level at the bin wall less than 1 milliroentgen per hour, a safe level for personnel.

Jan 1, 1973

By Vance G. Leak

A technique for recovering copper and steel from metallic scrap has been developed by the Bureau of Mines based on preferential melting in molten salt baths at 1,150° to 1,250° C, The molten salt, preferably barium chloride or calcium chloride, both minimizes oxidation of the metals and promotes heat transfer. Cleanest separations (0.01 percent copper remaining in iron) have been achieved by pretreatment (dipping or spraying) with sodium sulphate or sodium silicate, which alters and coats the surface of the iron to inhibit the alloying or brazing with copper. An economic evaluation of the process was carried out on six combinations of sweating media and inhibiting reagents. On the basis of the postulated model, a cost of about $0.20 per pound of copper recovered has been determined for the sweating treatment operation.

Jan 1, 1973

By Terry L. Muldoon

The Bureau of Mines conducted an investigation to quantify microphone response variations that could result when the microphone is worn by a worker, as with a personal noise dosimeter, and to suggest an optimum placement and orientation of the microphone for noise exposure measurements. Previous studies have shown no significant variations in a diffuse field. This investigation, therefore, was conducted in the free-field conditions of an anechoic chamber using an anthropometric dummy as a subject, and broad band noise as the acoustic stimulus. This investigation established that, in a free field, the wearer's body does significantly affect microphone response; the response variations are a function of azimuth, and location and orientation of the microphone. Results suggest that locating the microphone on top of the subject's shoulder, oriented parallel to the body axis, should yield data comparable to that obtained using a sound-level meter.

Jan 1, 1973

By Green R. E.

The removal of silica from commercial iron oxide concentrates by dissolution with sodium hydroxide was investigated by the Bureau of Mines as a means for producing supergrade concentrates. The effects of strength of solution, temperature, and digestion time on the extraction of silica were evaluated using eight iron oxide concentrates. Silica extraction from the eight concentrates was enhanced by autoclave leaching in the temperature range of 150° to 250° C and varied from 70 to 95 pct depending on the concentrate used. Superconcentrates containing less than 2 pct Si02 and more than 69 pct Fe were made only when magnetite concentrates were leached in the autoclave. The investigation showed that it is not difficult to obtain a supergrade product if the gangue is mainly quartz.

Jan 1, 1973