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By Earl L. Phillips

The Bureau of Mines conducted laboratory tests on samples of pozzolaniccement concrete to develop a low- strength backfill . Results show that support costs can be lowered by replacing a portion of the portland cement in mine backfill with pozzolan ( fly ash ) and lime . Unconfined compression tests on various ratios of fly ash to cement in 84 samples produced compressivestrength curves that can be used to estimate the best backfill mix for any mine .

Jan 1, 1964

Most laboratory sealant studies were carried out in 2.0 inch I.D. Plexiglas tubes of 9.0 inches height containing 4.0 to 4.5 inches reconstructed soil from an 0-8 or 8-16 inch soil horizon at the Lanse site. (When soil was used from the Kato site, the top soil horizon was approximately 0-4 inches. The 4-8 inch horizon was somewhat comparable to the Lanse 8-16 inch horizon.) A 20 mesh Saran or steel screen was placed over the rubber stopper with a bottom drain to a 100 ml measuring cylinder. In some earlier experiments a 1/2 inch bed of 1/4 inch pea-gravel was then added, but in later experiments this was eliminated as it showed no particular utility. Field soil samples collected by a shovel were stored in sealed containers and sieved through a 4 mesh screen just before use. (Moisture content was typically about 25% for A horizon soil and about 20% for B horizon soil.) The sieved soil minus roots was then added in increments of about 1 1/4 inches. Compaction was effected by dropping a weighted ramrod (1-7/8 inches O.D,) five times from a height of two inches. If about twenty tamps were used or if the soil columns were rapped vigorously while water-logged, compaction was high with no detectable percolation. Freezing such samples would then usually cause very slow percolation, e.g. 1-2 ml/day. Using this as a standard procedure, percolation flows were usually stablized after two to three days to rates of about 100 to 200 ml/hour. Percolate was recycled carefully to minimize disturbance of the soil surface. When percolation flows were about 100 to 200 ml/hour, various additives (sealants) were introduced to the moist column in two to three increments to maintain a slight head. Additive concentrations were usually 2-1/2% with some at 5% in earlier experiments. Typical use of 40 ml of 2-1/2% additive corresponds to 4400 lbs/acre. When no more additive was present as supernatent liquid, water washes of about 15 ml were then used several times followed by special additives as needed. More water washes were then used to maintain a head of about 1/2 inch. Percolate was collected in 100 ml cylinders to measure percolation rates in ml/hr. Turbid percolate was evaporated to determine amount of eluted latex. Percolate was sometimes checked for pH by Pan-pH Indicator Paper9,10 reading in 0.5 units. Surface tension measurements were sometimes made by a DuNouy tensiometer10 in experiments using a surfactant for pretreatment.

Jan 1, 1972

By A. G. Starliper

The report covers studies by the Bureau of Mines on the removal of metallic values in two waste products from the Longhorn tin smelter at Texas City, Tex. One product was a slag that contained tin, tungsten, iron, tantalum, and columbium. The other product was a spent acid solution that contained tin, tungsten, iron, lead, copper, zinc, and silver and that came from presmelting treatment of impure tin concentrates. Molten slag was treated with sulfur or sulfur compounds and with coke, calcium carbide, or gaseous reductants to form tin sulfide that volatilized from the charge and to reduce tungsten along with iron and silicon to form a carbon-bearing metallic layer. The metallic layer was treated by an oxidizing alkali roast and then was water-leached to extract the tungsten. The waste acid was used in other experiments to dissolve an iron-tin- tungsten alloy (hardhead) obtained by direct reduction of the slag. An insoluble fraction containing tungsten, silver, silicon, columbium, and tantalum was removed, and copper was cemented on metallic iron, Tin was recovered by cementation on zinc plates, and lead was precipitated by adding sulfate ion. Iron was precipitated by increasing the pH which left a solution containing principally zinc. Slabs of hardhead were electrolyzed in an electrolyte consisting of waste acid to plate out groups of metals at different pH?s. The time did not permit thorough exploration of this method of treatment.

Jan 1, 1962

By B. D. Nash

The Bureau of Mines continued its research into the recovery of fluorine by the phosphoric acid acidulation defluorination of phosphate rock concentrates. A small process development unit with a capacity of about 10 kilo-grams of charge per hour was operated, and concentrates from both Idaho and Florida were processed. Over 80 percent of the fluorine was evolved and recovered as a dilute fluosilicic acid solution. Phosphate extraction from the concentrates always exceeded 98 percent. The fluorine was converted to a synthetic fluorspar product (3CaFa?SiOa) suitable for use as a slag conditioner in electric furnace steelmaking operations.

Jan 1, 1977

A knowledge of the mechanics of wave propagation through the earth is essential if reliable communication systems are to be designed for coal mine environments. To obtain a reliable basis from which accurate propagation predictions could be drawn, a series of theoretical studies have been prepared for the US Bureau of Mines by Mr. Ramsay Decker of Spectra Associates, Inc. through a subcontract with Collins Radio Group. These reports formulate the analytical techniques from which we may derive frequencies and antenna configurations that yield the optimum signal-to-noise ratios over the greatest distances in mine environments. The reports of sections 2 and 4 deal with analytical techniques for determining the signal-to- noise ratio within a mine environment for loop-to-loop and line source-to-loop antenna con- figurations. The analytical results of these reports were then implemented into computer programs to obtain predictions concerning through-the-earth signal propagation. These preliminary predictions are based on noise data compiled by Bensema, Maxwell and Stone, and WVU prior to the extensive research conducted by the National Bureau of Standards (NBS). These initial measurements indicated a 20- to 30-dB lower noise level than that measured recently by NBS. The recent NBS data is that used by Collins in the final predictions. The following outline indicates the order and subject matter treated in the subsequent sections: Section 2 - Signal-to-Noise Analysis for Loop-to-Loop Mine Communications Section 3 - The Horizontal Electric Dipole Section 4 - Signal-to-Noise Analysis for Down-Link Line Source Mine Communications Section 5 - LF Communication Section 6 - The Application of Recent NBS Noise Data to Mine Communications Section 7 - Analysis of Mine Communication Propagation Programs

Nov 15, 1974

By D. H. Chambers, Arnold M. Lansche

Electro recovery by amalgam methods was investigated to determine the feasibility of recovering pure cadmium from cadmium sponge produced during purification of zinc electrolyte at electrolytic zinc plants . Actual material used in this work was air- oxidized cadmium sponge . An acid rinse and zinc displacement technique was developed to amalgamate this oxidized cadmium . ( In - plant use of the recovery process would probably not require this step because of the fresh state of the sponge . ) Zinc was completely removed from amalgamated sponge by selective oxidation with air . Zinc - free cadmium amalgam was circulated by an electromagnetic pump through an electrolytic cell where cadmium of 99.9+ percent purity was electrodeposited onto a rotating aluminum cathode . Polarographic methods were developed for determining cadmium and zinc in mercury and in sulfuric acid solution .

Jan 1, 1964

By R. W. Hiteshue, R. W. Fridy, W. Kawa

A study of the production of coronene , a high - melting ( 440 ° C ) , highboiling ( 525 ° C) , polynuclear hydrocarbon , was made by the Bureau of Mines to determine the maximum yield obtainable by the hydrogenation of coal and coalderived materials . Experiments were made with anthracite and bituminous coals and with asphaltenes and centrifuged residue obtained from heavy oil produced in a pilot plant by the hydrogenation of a bituminous coal at 2,000 psi and 480 ° C. With anthracite , yields of coronene of 0.5 to 0.7 wt pct of moistureand ash - free coal were obtained at 6,000 to 8,000 psi , 700 ° to 750 ° C , and a residence time of 30 minutes . With bituminous coal , yields averaging 0.4 wt pct of maf coal were obtained at 6,000 psi , 800 ° C , and 30 minutes ' residence time . With asphaltene and centrifuged residue , yields of less than 0.02 wt pct of maf coal were obtained at 6,000 psi , 700 ° C , and 60 minutes ' residence time .

Jan 1, 1964

By Paul M. Tyler

Graphite is an essential war mineral and for that reason has received much attention from the standpoint of national defense. During the World War the situation with respect to graphite supplies, though it never became acute, caused considerable concern. Even in peace time, however, graphite has aroused more interest than the actual size of the industry seems to warrant. Despite this wide interest the facts of the industry do not seem to be generally known. Often there has been an almost total disregard of the essential' economic and technical problems involved. Long ago Bastin3 made the following statement; in a Government' report: "To-day there are more abandoned mines and mills in the United States than the number in operation * * *. In the number of times' some of these properties have changed hands in the course of a few years, there is a record of misrepresentation and disappointment that can hardly be equaled in any other branch of mining; and many properties have been notoriously associated with stock manipulation of doubtful character." According to one authority fully 600 graphite mines have failed in the United States, and the record shows that of all these properties scarcely a score have ever succeeded in operating for as much as a year or two. More than 40 mines have been worked at various times in the State of New York alone and at least that many in Alabama. Throughout the country, in fact, there are scarcely a dozen States in which efforts have not been made at some time to exploit graphite deposits. At the present time the list of mines that can be classed as at all active is reduced to less than ten. Failures inevitably occur in all lands of mining, but the disheartening feature of the record of graphite mining in this country is that so few ventures have even paid back the money put into them and. that none has been a conspicuous success.

Jan 1, 1929

By W. W. Adams

"A recent paper prepared by the writer summarized the results of an analysis of the accident records of 34 metal mines for the calendar year 1925. The present paper summarizes the results of a similar analysis of the accident records of 59 coal mines for the same year. This summary is based upon reports furnished to the Bureau of Mines, Department of Commerce, by operating companies that par¬ticipated in the National Safety Competition of 1925.The purpose of the Competition was to establish the lowest accident-severity rate, thus showing the smallest loss of time from accidents in proportion to total number of man-hours worked. The reports covered all lost-time accidents that occurred during the year, that is, all accidents that disabled an employee beyond the day or shift on which the accident occurred. Detailed information for each of the 59 coal mines is given in the appended table. Each mine employed at least fifty men underground; over half of than employed more than 200 men underground. Hence the accident records should be typical of those of large-scale mining operations in general where the company is devoting special attention to accident-prevention work. The mines covered by the reports are situated in eleven States: Alabama, Illinois, Indiana, Kentucky, Maryland, Ohio, Pennsylvania, Tennessee, Utah, Washington, and West Virginia.A tabulation of the reports covering the 59 mines showed an accident-frequency rate of 123 per million hours of ""exposure* and an accident-severity rate of 10.214 per thousand hours of exposure3. The total volume of exposure or employment was 29,117,561 hours, representing the equivalent of work of 12,000 men for three hundred 8-hour shifts. The records covered employment and accident above ground as well as underground, although they did not include stripping or open-pit mining. Accidents during the year resulted in 33 deaths, 1 permanent total disability, 28 permanent partial disabilities, and 3,510 temporary injuries. These accidents represented a loss of tine equal to 297,417 man days. In arriving at this lost-time equivalent, each fatality and permanent total disability was weighted at 6,000 lost days (see footnote 3), as specified in the scale adopted by the International Association of Industrial Accident Boards and Commissions; permanent partial disabilities were weighted according to nature of injury, in accordance with the scale adopted by the :Board; temporary injuries were weighted according to the actual number of calendar days during which the employee was incapacitated as a result of the injury."

Nov 1, 1926

By K. K. Kelley, W. W. Weller

Heat capacity measurements of lead molybdate and lead tungstate were conducted over the temperature range from 51 ° to 298 ° K. The entropies were found to be S298.15 = 39.7 ± 0.5 cal / deg mole for lead molybdate and S298.15 = 40.2 ± 0.5 cal / deg mole for lead tungstate . The entropy values were combined with other pertinent data to obtain the entropies of formation of the two compounds from their constituent elements and oxides .

Jan 1, 1964

By Oren C. Baptist

Umiat field contains the largest accumulation of oil discovered so far in Naval Petroleum Reserve No. 4 in Arctic Alaska. The Umiat anticline was tested with 11 wells; 6 produced oil in varying quantities. Behavior of the wells during testing was unpredictable. For example, one well was abandoned as a dry hole after all tests failed to recover any oil, yet an offset well, only 200 feet from the dry hole, produced 400 barrels of oil a day. The main oil reservoirs are less than 1,000 feet deep and are in the permanently frozen zone (permafrost). Reservoir pressures are low, and most primary production will be by expansion of gas-in-solution in the oil. Because of the unusual reservoir conditions and the difficulties encountered in drilling and completing the wells, the Department of the Navy asked the Federal Bureau of Mines to make laboratory studies of the reservoir sand to determine the cause of well plugging and to provide laboratory information, to be used as an aid in estimating oil recovery from frozen reservoir rocks under solution-gas expansion from low-saturation pressure conditions.

Jan 1, 1960

By John A. Johnson

Conclusions regarding the use or omission of stemming in blasting have not peen reached, pending completion of all aspects of this investigation. The results from the dust phase of this study on six classes of stemming prove that the kind of stemming affects the amount of dust produced from blasting. In previous work at the Mount Weather testing adit it was demonstrated that blasting produces the highest dust concentrations of any of the mining processes.5/ Under the conditions prevailing at the Mount Weather testing adit, the average of all rounds having a break of at least 95 percent showed that the least amount of dust was produced when no stemming was used.

Jan 1, 1940

By E. S. Longfellow, S. H. Katz

Poisonous hydrocyanic acid gas (HCN) is sometimes evolved in dangerous quantities from cyanides used in metallurgical and chemical operations. This gas is much used for fumigating buildings, ships, greenhouses, and such commodities as grain and cotton to destroy rats, mice and insect pests. Wherever cyanide fumes are evolved, thorough ventilation is necessary in order to render the sur- rounding air safe to breathe. Many persons have been killed by entering tanks and fumigated places too soon, and a simple test for this gas would promote safety. In view of the need for an easy method for quantitatively determining HCN in air, the three color reactions used originally for testing HCN in solution tions *** were modified and adapted. The reactions employ (1) picric acid (CH(NO2)3OH) which is yellow but combines with hydrogen cyanide to form a red- purple dye, isopurpuric acid****; (2) phenolphthalin (CH1604), which is a reduc- tian product of the phenolphthalein (CH4) used for acid indicator, this colorless substance is oxidized***** by presence of HCN to pink colored phenolph- thalin; and (3) guaiacum which oxidized from colorless to blue******. Phenolph- thalin and guaiacum require the presence of copper compounds which catalize the color formation by reduction of cupric cyanide. The chemical processes involved *Associate physical organic chemist, Bureau of Mines, Department of the Interior. **Assistant gas chemist, Bureau of Mines, Department of the Interior. 2014 20 *** Kohn-Abrest, E., Notice toxicologique sur les gas: Arnales des Falsifica- tions, vol. 8, 1915, pp. 215-35. (Tested air with picric acid and guaiacum papers). **** Élasiwietz, H., Ueber eine neue Zersetzungsweise der Trinitrophenylsaure: Anal. der Chemie, vol. 110, 1859, pp. 289-303. ***** Weehuizen, F., Phenolphthalin as reagent for HCN: Pharmaceutrisch weekblad, Utrecht, vol. 42, 1905, pp. 271-2. Abstract, Jour. Chem. Soc., vol. 88, part 2, 1905, p. 489. ****** Schonbein, C. F., Ueber den thatigen Zustand der Helfte des in dem Kupfer- oxydenthaltenen Sauerstoffs und ein darauf beruhendes hochst empfindliches Reagens auf die Blausaure und die loslichen Cyanmetalle: Jour. fur. Praktische Chemie, vol. 106, 1869, pp. 263-70.

Jun 1, 1923

By R. D. Haynes

Coal, gas, and oil in many geological formations of the Eastern United States are intimately associated but have traditionally been recovered independently of each other. Oil and gas wells, however, are often spaced sufficiently close to cause the subsequent loss of up to 50 percent of the recoverable coal in the form of pillars or barriers left for mine safety purposes. A long-range planning technique was devised for exploiting oil and gas wells simultaneously with the mining of coal to recover the maximum fuel potential of the formations. Planned plugging of oil and gas wells, determined partly from production predictions via decline curve analysis, is coordinated with a mine development plan to achieve maximum coal recovery and reduce overall production losses of gas and oil due to plugging of the wells.

Jan 1, 1973

By P. C. Good

The Bureau of Mines conducted a laboratory investigation of a sinter-leach method to recover aluminum and fluorine from waste carbon potlining residues from secondary cryolite recovery operations in aluminum reduction plants. After removal of carbon by burning, the residue was sintered at 900° to 1,100° C with silica and N2CO3, then crushed and leached with dilute NaOH solution, dilute Na2C03 solution, water, or water containing residual Na2O which remained in the sinter after reaction and decomposition of Na2CO3. Over 90 percent of the contained aluminum and up to 87 percent of the contained fluorine were extracted from this waste product in the form of a mixed alkaline solution. Treatment of the alkaline solution with CO2 yielded a white precipitate containing 89 percent of the original aluminum and 61 percent of the original fluorine as a mixture of synthetic cryolite and alumina, together with a variable excess of soda.

Jan 1, 1969

By A. W. Fahrenwald

Many factors enter into the efficient operation of the reciprocating type of gravity concentrator. Earlier investigators who studied these factor invariably used natural (crushed ore) products for their experiments, but in the present study synthetic products were used. The variables considered were (1) specific gravity of the sand grains, (2) size of sand drains, and (3) shape of sand grains comprising the table feeds. It is recognized, also, that the percentage relationship of the different kinds of grains is a factor affecting results. This factor is variable in one group of experiments but is thereafter kept constant.

Jan 1, 1929

By J. P. Bennett

Based on previous Bureau of Mines research indicating that improved high-temperature properties could be achieved for periclase refractories through chemical additions, the Bureau investigated the properties of full-size bricks produced from chemically modified periclase refractory grains and the suitability of making such chemical additions to Mg(OH)2 slurries prior to production of the periclase grains. In full-size brick testing, strength values, both hot and cold, for the optimized bricks were superior to those for a commercial 98-wt-pct-MgO refractory. The best results were obtained for a natural magnesite with an adjusted CaO:Si02 (C:S) ratio of 3.0 and a 1.0-wt-pct addition of Zr02 and for a seawater periclase with an adjusted C:S ratio of 2.5 and a 0.5-wt-pct addition of Mn02. For samples produced from chemically modified Mg(OH)2 slurries, additions of both Mn02 and Zr02 and an increase in C:S ratios produced significant increases in hot flexural strength, similar to those resulting from chemical additions made to periclase grains. The most effective modifications were additions of Mn02 to brine-derived periclases having a C:S ratio adjusted to 3.0. These results on chemically modified magnesia refractories indicate that such material could potentially substitute for magnesiachrome refractories containing imported chromite.

Jan 1, 1984

By John M. Gomes

Two molten salt systems were evaluated as electrolytes for the repetitive recovery of tungsten from tungsten oxide (W03) made by calcining commercial-grade ammonium paratungstate. Using a sodium chloride-sodium fluoride-potassium aluminum tetrafluoride electrolyte at 800° C, 1 pound of 99.8 percent tungsten was recovered for each 2.7 kilowatt-hours of energy consumed. The metal contained 1,100 ppm carbon, was in dendritic masses of spherical grains, and had an apparent bulk density of 5.41 g/cm3. T ngsten of 99.9 percent purity was won from a sodium pyrophosphate-sodium tetraborate-sodium chloride electrolyte at 1,000° C; 6.0 kilowatt-hours of energy was consumed for each pound of metal recovered. The metal contained 120 ppm carbon, was in dendritic masses of hexagonal acicular crystals, and had an apparent bulk density of 7.25 g/cm . Each metallic impurity--aluminum, calcium, copper, iron, nickel, and silicon--in the two tungsten products was 16 ppm or less.

Jan 1, 1966

By F. S. Wartman

The presence of magnetite, either dissolved or suspended as solid crystals, in slags from the copper reverberatory furnace is a frequently mentioned cause of an abnormally high copper content in those slags. The presence of this oxide in the slag is to be expected, since it is present in appreciable amounts in both converter slag and roaster calcine which comprise a considerable proportion of the furnace feed. Magnetite is also a product of some of the furnace reactions. These abnormal losses result in several ways. Magnetite is supposed to favor the formation and retention of copper ferrite, in the slag. Crystals of solid magnetite suspended in the slag are objectionable-because they make the slag less fluid and often entrap globules of matte. Frequently these crystals settle into a layer at the slab-matte interface which may have such mechanical strength as to create a false bottom and interfere with furnace operation by preventing separation of matte from slag. Magnetite may, by crystallizing on the furnace bottom, build the bottom to such a level that the furnace can no longer be operated.

Jan 1, 1928

By R. F. Abernethy

A chemical method of determining microgram quantities of arsenic in coal was investigated by the Bureau of Mines to supplement a semiquantitative spectrographic method of determining arsenic in coal ash. In accordance with a method recommended by the International Organization for Standardization, 1-gram samples of coal are decomposed by wet oxidation with boiling sulfuric acid (H2S04) and nitric acid (HN03) to remove the organic matter. After heating to fumes of SO3 to remove HN03, the arsenic is separated as arsine by the action of zinc in H2S04 solution. The arsine is absorbed in dilute iodine solution in which the arsenic is determined colorimetrically by the molybdenum-blue reaction. Two modifications of the method for obtaining the arsenic in solution, in addition to the wet oxidation method, give satisfactory results. The modifications are (1) furnace ashing with MgO added to the coal, followed by treatment with H2S04, and (2) extraction of arsenic from the coal by dilute HNO3 without ashing. Float-and sink-tests show that arsenic is associated mainly with mineral matter in the three coals examined. High-temperature ashing tests show that very little arsenic is volatilized from coal ash below 1,000° C, but it is virtually all removed from the ash at 1,300° C.

Jan 1, 1968