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By C. W. Schultz

The vapor pressure of manganese in equilibrium with a series of liquid iron-manganese alloys was determined by the carrier gas method over a broad range of alloy composition. From these data the activities of manganese in the iron-manganese system were calculated. The system appears to be ideal.

Jan 1, 1966

By Foster Fraas

A separator for minerals of low magnetic susceptibility and fine particle size in a water suspension is described. A ring-shaped matrix of ferromagnetic fragments rotating so as to pass successively through magnetic-field and field-free regions provides for the separation. Application is illustrated in the separation of hematite and ilmenite from quartz.

Jan 1, 1966

By Jr. Koch

Statistical methods applied at the Bureau of Mines Denver Mining Research Center to data from metallic ore bodies were used to evaluate lignite reserves from core data and to predict the extent of lignite horizons in some Texas lignite beds. Six lignite seam units were studied using data from 361 drill holes. The data indicate a total of 214.2 million tons of lignite in the area examined, and probable reserves of 113 million tons in an area 2,000 feet beyond the limits established by the drill holes. It was demonstrated that lignite reserves present in lenticular beds could be reliably determined by statistical techniques, and that core drilling could be optimized to maximum information with minimum drill holes. The technique described is applicable to other coal beds.

Jan 1, 1966

By Jr. Jacobson

Thermal reactions of l-methylpyrrole, l-butylpyrrole, and l-isopropyl-pyrrole were investigated by a flow method in the temperature range of 4500 to 5750 C. Those of I-butylpyrrole and l-isopropylpyrrole were also investigated in the 3400 to 4000 C range in a static system. The I-substituted pyrroles isomerize by an irreversible reaction to 2-substituted pyrroles. A reversible isomerization reaction shifted the alkyl group from the 2-to the 3-position on the pyrrole ring. All of the isomerization reactions are homogeneous, unimolecular, nonchain, first-order reactions having similar mechanisms and transition states. There is decomposition and cleavage of the longer alkyl side chain when it is in either the 2-or 3-position giving, as products, pyrrole, 2-and 3-methylpyrrole, 2-and 3-ethylpyrrole, pyridines, and hydrocarbons. The decomposition reactions appear to be by free-radical mechanisms. Pyridine homologs are formed by the expansion of the alkylpyrrole: butylpyrrole produces pyridine, and isopropylpyrrole produces 3-methylpyridine. Approximate Arrhenius equations are given for the formation of the decomposition products.

Jan 1, 1966

By A. F. MacDonald

The rugged foothills of the Allegheny Mountains in Washington County, Southwestern Pennsylvania, lend their terrain very well to the use of aerial tram systems to carry refuse from Bethlehem Mines' two preparation plants to disposal areas some distance from the plant site. Bethlehem Nines Corporation has three deep mines in this area, all of which are mining the Pittsburgh Coal Seam, The raw coal is prepared for metallurgical use in a preparation plant at each mine, Trio of these preparation plants, Mine No, 51, Ellsworth and Mine No. 58 Marianna, use aerial tram systems to dispose of reject material.

Jan 1, 1966

By R. O. Vernon

The Florida Peninsula has existed as a part of a much broader plateau, since at least the Early Cretaceous. This plateau, the Floridan Plateau, now consists of the present peninsula and a broad submerged shelf of equivalent size extending the length of the state and out into the Gulf of Mexico. Florida Peninsula was separated from the mainland United States by a negative area called the Suwannee Straits. To the south of this feature existed an environment similar to today?s Bahamo Banks where very pure calcium and magnesium carbonates with associated evaporites were deposited. Thus the Eocene and Oligocene contain little or no quartz sand or clay minerals except in the Panhandle west of the Suwannee Straits where some clastics were contributed by rivers from the north.

Jan 1, 1966

By T. C. Crosby

Grinding has a marked effect on concentrator recovery and opera- ting cost, improved operation through automatic control can enhance plant performance. The correct application of automatic control can only be accomplished after the basic process variables and their effect on mill operation have been defined. This paper develops a control system for a closed circuit grinding system. Typical control systems such as feed, water flow, level and circulating load are discussed. A method of determining controllability is outlined using the calculated reaction curve technique. Various successful methods of automatic grinding control applications are discussed and future possibilities are outlined. Although this paper primarily deals with closed circuit wet grinding circuits, the principles involved can be readily applied to other processes.

Jan 1, 1966

By Albert F. Baker

Techniques were developed and circuitry was assembled for measuring the total and volume resistances to the flow of electric current through solid specimens of anthracite. The two-, three-, and four-terminal test methods demonstrated the extreme sensitivity of resistivity to differences in anthracite characteristics and showed response to changes resulting from variations in structure, temperature, and moisture content.

Jan 1, 1966

By Jr. Sharkey

The Bureau of Mines investigated gases from flash and laser irradiation of Pittsburgh seam (hvab) coal to determine the action of high temperatures on coal. Temperatures in excess of l,000° C were reached with both types of irradiation. Craters about 300 microns in diameter were produced in the coal with millisecond pulses from the laser unit rated at 1.7 joules' output. Gaseous products from laser and flash irradiations in vacuum contained 21 and 8 percent acetylene, respectively. Diacetylene, vinylacetylene, and other products to molecular weight 130 were indicated in the mass spectrum of the gas from the laser study. Single experiments were also conducted in which the laser energy, particle size of the coal, and atmosphere were varied. The results indicated that the distributions of products obtained from the flash and laser irradiations of coal were different from that produced in high-temperature carbonization.

Jan 1, 1966

By Peter A. Cain, John C. Folinsbee

"A 4-ft.-diameter shaft has been drilled to a depth of 2,790 ft. in strong, hard, basic Precambrian rocks at Lynn Lake Manitoba. This was done on the property of Sherritt Gordon Mines Limited for the purpose of ventilating and developing the ""N"" orebody, which is located approximately 4,000 ft. south of the Farley shaft.The drilling was done under contract by two drilling companies. Peter Bawden Drilling (1964) Limited drilled the initial 12:1,4-in. pilot hole to a depth of 3,000 ft. Shaft Drillers Limited of Canada then reamed the hole to 4 ft. in diameter to a depth of 2,790 ft. At this point, the reaming was stopped because of the difficulty in passing a change in direction in the line of the pilot hole. The hole was completed by driving a raise 200 ft. from the 3000 level to the bottom of the 4-ft. hole using an Alimak raise climber.Cuttings from the reaming operation were directed into the 12:1,4-in. pilot hole, where they fell to the 3000 level and were removed by a mucking machine and standard mine development cars.The elapsed time from the start of the pilot hole to the completion of the reaming operation was ten months, with an average advance of 279ft. per month. There was a two-month delay between the completion of the pilot hole and the start of the reaming operation.The 12:1,4-in. hole was drilled in an elapsed time of 45 days from the time of setting up the rig. The average advance per day was 66.8 ft.The reaming operation was done in an elapsed time of 194 days. A one-month delay required to repair damaged equipment left 163 days for the drilling and setting-up operation, for an advance per day of 17.1 ft."

Jan 1, 1966

By J. E. Zeilinger

The technical feasibility of using energy from explosive ignitions of coal dust to pump water was .demonstrated in an exploratory investigation. Ignition of small amounts of pulverized coal that were dispersed in air over columns of water pumped up to 5.3 gallons of water per cycle when operated against a head of 30.75 feet. Water displacement was accomplished by either manual or automatic operation through a single cycle, and by automatic operation through a continuous series of cycles of I-minute duration. Operating through single cycles, slurries containing up to 3 pounds of coal and 4.6 gallons of water were also pumped. Possible uses of an efficient coal-fired pump would include pumping water for irrigation purposes, removing water from mines, transporting coal from mines in the form of a slurry, and pumping water to elevated reservoirs at electric powerplants so that it could be used to generate electricity during peak periods of demand.

Jan 1, 1966

By Alvin Kaufman

To aid industry and Government in planning water developments the Bureau of Mines in 1963 canvassed mineral producers to determine water use in 1962. Water use by the mineral industry comprises only 2 percent of the water withdrawn by industry as a whole. The major water-using mineral industries are natural gas processing, phosphate rock, sand and gravel, and iron ore. Analysis indicated the following conclusions: 1. Total water use and new water intake is dependent on the quantity of material processed and the process water requirements of the particular industry or commodity. 2. Recirculation is dependent on the processing requirements of a particular commodity, the manner in which the water is used, cooling and condensing requirements in certain large industries, the quality of new water intake, and the need to treat new and discharged water. 3. Consumed water is dependent on the quantity of water recirculated, the temperature and humidity in the area, and the proportion of water used for cooling and condensing. 4. A threefold increase in water use by the mineral industry by 1985 is forecast.

Jan 1, 1966

By P. E. Churchward

The Bureau of Mines developed a process using amines for recovering tungsten as ammonium paratungstate from alkaline leach liquors without producing synthetic scheelite as an intermediate product. Over 90 pct of the tungsten in low-grade scheelite or ferberite concen-trate was recovered as ammonium paratungstate by (l) autoclave leaching the concentrate with Na2CO3, (2) solvent extraction of the acidified leach liquor with kerosine solutions of either a quaternary amine (Aliquat 336) or a primary amine (Primene JM-T), (3) stripping the tungsten values from the quaternary amine with ammoniacal NH4C1 or from the primary amine with NH4OH, and (4) crystallization of ammonium paratungstate from the strip liquor. Reagent consumption in pounds per pound of W03 recovered was, for the quater¬nary amine, 3 Na2CO3, 3.5 H2SO4 , 2.2 NH4Cl, 1 NH3, and 0.4 glacial acetic acid; for the primary amine, it was 3 Na2CO3, 3.5 H2SO4, .06 NH4Cl, and 0.9 NH3. Both reagents extract molybdenum along with tungsten. Silicate and phosphate are partly extracted and contaminate the product; leach liquors containing these impurities require preliminary purification.

Jan 1, 1966

By V. S. Gupt, W. H. Somerton

Rock may undergo great changes in physical properties when heated to high temperatures and then cooled, The temperature and intensity of reactions causing rock alterntiorl.s can he controlled by introducing certain chemicals during heat treament. Three typical outcrop sandsone samples were saturuted with common salt solutions, then heated to several maximum temperatures. After cooling, it was found that per-rrreuhilities had increased much more for salt-saturated samples than for samples not saturated with salt but heated to the same temperatures. This was only true, however. for samples heated above the melting points of the particrrlar salts. Potassium chloritle was particularly effective with Bandera sandstone. Samples saturated with potassium chlorirlr. solution and heated to 900C showed an 11-fold increa.se in perrrieahility. Samples without potasrirdrn chloritle but heated to the .same temperature. showed only a 2.7-jold incresre in permecahility. In application, it seems possible that injecting chemicalc into the formations from a wellbore followed by applying intensive borehole heating might promote reactions which would greatly improve permeability of the formalions. INTRODUCTION Great changes in the physical properties of rocks which have been heated to temperatures in the range of 600 to 800C have been reported earlier. Permeability increases of 50 per cent, and equivalent decreases in sonic velocity and breaking strength have been observed. Although there might be some suppression of certain reactions responsiblc for these changes when rock samples are heated under simulated reservoir pressure conditions. recent work has shown that these are more than offset by the increased importance of other reactions at high pressures. The reactions considered responsible for alteration of rock properties by heating include differential thermal expansion. dehydration, phase changes and dissociation of mineral constituents. Ceramists have long known that temperatures at which reactions occur can be raised or lowered by the presence of certain impurities in the sys. tcnl. Thus the possibility exists that by saturating rocks with appropriate solutions. desired reactions might be accelerated and unwanted reactions might be suppressec! when the rock is heated. Purpose of the present work was to investigate the effects of several common salts on the thermal alteration of sandstones. Types of reactions which might occur are reviewed and the findings of a number of thernlochemical alteration tests are presented. THEKMOCHEMICAL ALTERATION OF SANDSTONE MINERALS The most abundant constituent of most sandstones is quartz. Quartz can exist in at least eight different forms, but in the temperature range of immediate interest (to 900C) only two forms are of importance—alpha quartz below 573C and beta quartz above this temperature. Although the alpha-beta inversion of quartz is very important in thermal alteration of rocks. it is not particularly important here because the inversion temperature cannot be changed significantly by the presence of impurities or by the application of pressure. The transition temperature of quartz to tridynlite is 867C. but the transition is very sluggish. Tridymite is considered to be a metastable transition phase between two stable phases: quartz?cristobalite. However. the transition temperature for tridymite to cristobalite is 1,470C.4 The quartz-tridymite-cristobalite transition can be accelerated substantially by the presence of fluxing agents. Finely divided calcium, magnesium and titanium oxides accelerate the conversion while A12O may retard it. A Mixture of NaCl and CsCl reduces the temperature for cristobalite formation by as much as 420°C. Feldspars constitute the second most important mineral in sandstones. The melting points of feldspars range between 1,000 and 1,700°C depending upon the variety. No information available indicated any important role of fluxing agents in the thermal alteration of this group of minerals. Carbonate minerals are subject to dissociation at temperatures within the range of the present investigation. The dissociation of magnesite can start at a temperature of 373°C, but the reaction is sluggish and might not occur untll a temperature of 500°C or ,higher is reached. Dolomite dissociates in two stages at 500°C and 890°C, whereas calcite dissociation temperature is about 885C. Because CO2 is released in the dissociation of carbonates, ail such reactions are somewhat dependent upon CO2 partial pressure. In the absence of CO: in the surrounding atmosphere, the dissociation of calcite starts at 500°C.However. when 1 atm of CO surrounds the sample, the dissociation does not start until 900C. The other carbonates are apparently much less sensitive to a change in partial pressure of CO2. The aragonite calcite transformation can occur an!. where within the temperature range of 357 to 488°C. depending upon the presence of impurities such as barium. strontium. lead and perhaps zinc. The differential thermal analysis (DTA) curves of both magnesitc and dolomite vary with the presence of 'impuritics. The presence of iron in particular seems to affect the magnesitc DTA curve

Jan 1, 1966

By L. C. Marchont

This Bureau of Mines report tabulates data on nitrogen-gas reservoirs and isolated occurrences of inert gases in several Williston basin oilfields. Recoverable reserves of nitrogen gas in the Minnelusa nitrogen interval within the areas of five oilfields on the Nesson anticline in North Dakota are estimated at about 1.27 trillion standard cubic feet, based on computer analyses of logs from over 300 wells. This volume of nitrogen represents a large source of high-pressure inert gas and warrants consideration of possible application in oil-production operations. Drill-stem tests made in two of the fields indicated that nitrogen can be produced at rates up to 28 million cubic feet per day.

Jan 1, 1966

By Joseph J. Garbarino

World demand for phosphate fertilizers has grown at an average annual rate of between 6 and 7 per cent over the past 10 years. In the next five years world demand is expected to at least continue to grow at that rate. Also, the continued need for improved fertilizer materials, coupled with improvements in fertilizer technology, have placed added importance on the use of phosphoric acid as a starting material for high analysis phosphate fertilizers. This demand for phosphates and phosphoric acid must be met by increased production. Increased phosphoric acid production also brings increased demand for chemical processing agents including foam control agents. We at Arizona Chemical Company have closely followed the phosphate fertilizer industries needs. Arizona Chemical Company has been an important supplier of flotation agents to the phosphate industry, primarily from its Panama City, Florida plant. We have also recognized the important role played by foam control agents in the wet-phosphoric acid manufacturing process. We feel it is the responsibility of the supplier of foam control agents to offer specifically designed products that are highly efficient and economically useful. The difficulties involved in evaluating foam control agents in the plant are recognized. Owing to the large number of variables present, and the difficulties in controlling these variables during the period of a plant trial, plant evaluation of a large number of foam control agents is impractical. We have attempted to develop a practical, reproducible, and yet rapid, laboratory evaluation test which correlates with plant performance.

Jan 1, 1966

By H. J. Coleman

Knowledge of the types of naturally occurring sulfur compounds in petroleum is of both theoretical and practical interest to petroleum chemists and geologists. This knowledge has been extended by the identification of 77 sulfur compounds, including 36 thiols, 23 chain sulfides, and 18 cyclic sulfides in a 111° to 150° C boiling range distillate of Wasson, Texas, crude oil. The characterization procedure used in separating and identifying these compounds included isothermal distillation, vacuum fractionation, liquid-solid chromatography (alumina adsorption), chemical treatment, gas-liquid chromatography, microdesulfurization, and infrared analysis. The procedural steps described represent a systematic method of sulfur compound analysis considered applicable for determining the nature and concentration of the sulfur constituents present in any straight-run petroleum distillate of the above-boiling range.

Jan 1, 1966

By James W. Myers

The Bureau of Mines studied factors affecting ignition of coal mine refuse and on methods for control of burning. Laboratory experiments showed that air permeates more readily through segregated than through nonsegregated refuse and that air permeability is greater through coarse than through fine particle refuse. Minus 3-1/4-inch refuse ignites spontaneously more readily than minus 1/4-inch refuse. The burning of a 1,000-pound conical coal pile was con-trolled by capping with an 18-inch-thick layer of minus 1/4-inch refuse containing 37 percent combustible. In field trials, the burning of refuse at operating mines was controlled by capping with a layer of fine refuse. Water, applied as a spray or by injection, quenched surface flames and cooled the burning waste. Inspection of refuse piles at operating mines showed that the spontaneous ignition tendency is affected by the exposed surface relative to the total volume and the segregation of particles during dumping.

Jan 1, 1966

By Jerry W. Ramsey

The Bureau of Mines studied two Pennsylvania anthracites using low-temperature carbon dioxide adsorption. A modified form of the Brunauer-Emmett-Teller equation was used to calculate specific surface areas. Two mesh sizes of each anthracite were used to determine how gamma irradiation at 106 and 108 rads, both in vacuum and in the presence of air, affected the carbon dioxide surface areas. Results show that anthracites have a system of pores that are essentially all interconnected rather than isolated; that anthracites differ from one another in specific surface, which may correlate with density; and that irradiation in vacuum has no discernible effect on specific surface of anthracite, but irradiation in air does produce changes in specific surface.

Jan 1, 1966

By F. E. Griffith

Cost data are given for five methods of secondary backfilling of strip mines previously partially backfilled. The operations were conducted in north-central Pennsylvania; an average of 600 linear feet of highwall were backfilled in each trial. Major obstacles and the relative merits of the methods are discussed.

Jan 1, 1966