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By E. J. Murphy

The Bureau of Mines developed a fast, reliable modification of the Griess-Ilosvay procedure suitable for field analysis for NO2 in the fumes from explosives. Known concentrations of NO2-air mixtures were analyzed for the nitrous acid or nitrite formed in the reaction with three Griess-Ilosvay-type reagents by diazotizing and coupling. Comparison was made of the Rider-Mellon, Saltzman, and Patty-Petty procedures; the three procedures are in agreement if sufficient time of contact between NO2 and the reagents is allowed. In experiments to obtain an accurate factor for converting NO2 to nitrite, overnight contact was allowed in order to be sure conversion was complete. The factor was found to be 75 percent with a standard deviation of ±3.2. Low and erratic results were found using either the Saltzman or Patty-Petty reagents as absorbing liquids unless several hours' contact was allowed. If dilute NaOH solution was used as the absorbing liquid instead of a Griess-Ilosvay-type reagent, 92 percent of the overnight conversion factor was found after a 3-minute shaking time and a la-minute standby time. The Saltzman reagent was preferable for fieldwork with the dilute NaOH solution as the absorbent because of its easy application, rapid reaction, and intense color even at low NOB concentrations.

Jan 1, 1967

By C. F. Ellis

Interest in the composition of automobile exhaust gases has been greatly accelerated by recent studies that have indicated that these gases contribute to smog formation in urban areas. Several analytical methods have been published for the analysis of the hydrocarbons in the exhaust gases, but similar information has not been published on the analysis of the oxygenated compounds. This report presents procedures for chemical analyses of certain oxygenated compounds, procedures for sampling the exhaust gases for these analyses, and the analytical results of some experimental work in which these procedures were used. A stationary 1956 model, 170 horsepower, V-8, dynamometer-mounted engine, operated to simulate vehicular cruise conditions, was used for the study. Exhaust gases produced from a regular-grade Midcontinent gasoline during 15-40- , and 60-mile-per-hour cruise operations were analyzed by chemical methods for formaldehyde, total aldehydes, total carbonyls, total alcohols, carbon associated with the oxygenated compounds, and the oxides of nitrogen. Experimental results indicate: 1. The range of concentrations of the total of the functional groups of oxygenated compounds, expressed as moles per million moles of water-free exhaust gases, is about 90-100; the concentrations increase with engine speed. 2. Aldehydes comprise about 80-90 mole- percent of the total of the oxygenated groups, and formaldehyde accounts for about 50 mole-percent of the total aldehydes. 3. The order of magnitude of the concentration of the carbonyls is the same as that for the aldehydes, indicating that ketones are not a major group. A colorimetric test indicates that methyl ketones Constitute about 2 mole-percent of the oxygenated compounds.

Jan 1, 1961

By R. L. Montgomery

The heats of formation of lanthanum sulfate and the enneahydrate are -939.8 ± 3.1 and -1,587.1 ± 3.2 kcal. per mole, respectively. The heat of hydration is -32.5 ± 3.5 kca1. per mole. These values were obtained from heat-of-solution measurements of lanthanum oxide and salts. Low rates of solution precluded more accurate determinations of the thermal data. The heat of formation of the chloride was similarly observed to be -256.18 ± 0.28 kcal per mole. Heats of solution and combustion of lanthanum metal yield mutually concordant results, and earlier discrepancies reported in the literature may be ascribed to impurities.

Jan 1, 1959

By G. W. Birge, D. E. Wolfson, J. G. Walters

Seventeen samples were carbonized by the BM -AGA pilot - plant test method and in industrial ovens . Chemical and physical properties of the samples were determined , and the physical properties of the cokes prepared by the two methods were compared . Since the capacity of the plants from which these samples were obtained is about 30 percent of the 1959 total for the United States , the data given in this report are indicative of the chemical and physical properties of blends used to produce industrial cokes and the acceptable chemical and physical properties of the resultant coke .

Jan 1, 1964

By J. L. Shultz

Mass spectrometric analyses were obtained for naphthalene and anthracene oils, heavy creosote, and three fractions of a pitch. The average molecular weight, aromaticity, and mean structural unit were determined for each fraction. The investigation of these fractions of coal tar has resulted in semiquantitative data for 38 structural types and carbon number distribution data for their alkyl derivatives. The molecular weights of 10 of these structural types indicate ring systems not previously reported in products from high-temperature carbonization of coal. Two of these structures are poly-nuclear aromatic hydrocarbons, two are oxygen-containing compounds, one contains sulfur, and five are nitrogen-containing compounds.

Jan 1, 1967

By J. L. Reuss

The Bureau of Mines investigated the technical feasibility of smelting copper concentrates containing chalcocite (Cu2S) and native copper using nonpyritic sulfur-bearing materials to aid matte formation. The procedure consisted of combining various proportions of commercial chalcocite concentrate, smelter slag, fluxes, and matte-forming constituents to produce charges of comparable compositions. The mixtures were charged in fire-clay crucibles and smelted in an induction furnace at 1,300° C. The research proved that either sulfur or gypsum can replace pyrite as a matte-forming material, and that gypsum produces an exceptionally high-grade copper matte. The addition of small quantities of metallic iron to the nonpyritic smelting charge furthers the removal of sulfur, improves the recovery of copper, and makes it possible to utilize gypsum as the exclusive flux and matte-forming ingredient, thereby eliminating the necessity of adding limestone.

Jan 1, 1968

By G. H. Keith

A vanadium-base alloy consisting of the following elements in weight-percent--molybdenum, 20; titanium, 10; carbon, 0.1; silicon, 0.5; and yttrium, 0.5--had exceptionally high strength at temperatures up to 1,200° C. This alloy was capable of fabrication to sheet of ~ 1 mm thickness by a combination of hot swaging and hot and warm rolling. In the warm-rolled condition at ambient temperature, its ultimate tensile strength was 1,205 MN/m2. The strength at 1,200° C was 150 MN/m2. Within the temperature range of 25° to 1,200° C, the ductility of the alloy as measured by elongation increased from 4 to >90 percent. Strengthening was achieved by both solid-solution and dispersed-phase mechanisms. Alloys of 20 percent molybdenum and 10 percent titanium were stronger than the other molybdenum-titanium alloy compositions tested. Strength was increased 15 percent in the temperature range of 25° to 800° C, with no accompanying loss in ductility, by the addition of 0.5 percent silicon. Workability was improved by additions of 0.25 and 0.5 percent yttrium.

Jan 1, 1970

By James Paone

The Bureau of Mines made drillability studies with impregnated diamond bits in the laboratory on 7 rock types and in the field on 21 different rock types. Results indicate that drill parameters of rotational speed, thrust, and torque must produce sufficient applied forces to induce stress levels that cause continuous failure in rock to achieve efficient penetration rates. Higher rotational speeds appear to be more effective in drilling relatively harder rocks, although the increased speed causes more bit wear; increases in thrust result in higher drilling rates but not linearly; and up to a critical value a linear relation exists between torque and penetration rate for a specific rock type. Penetration rates with impregnated bits show a trend similar to that obtained with surface-set bits for rock under 25,000 psi compressive strength.

Jan 1, 1966

By John D. Prater

Thallium is one of the rarer metals that has come into commercial importance in recent years. Although the element was first reported by Crookes in seleniferous deposits in lead chambers of a sulfuric acid plant in the Harz Mountains of Germany, it had no commercial significance until about 190O because of the high cost of extraction. Thallium occurs widely in the earth's crust but is found in such low concentrations that it is recovered only as a byproduct from processing other elements. There are no domestic ores of thallium; the entire output in this country is supplied by the American Smelting & Refining Co. as a byproduct of its cadmium operations at Globe, Colo. Thallium also is recovered from the flue dusts of sulfuric acid works in which thallium-bearing materials are used and as a byproduct of the lithopone industry. This paper describes methods for recovery of thallium from 'white arsenic" and lead Cottrell-precipitator dust of the American Smelting & Refining Co., lead smelter, Murray, Utah. Owing to an enlarged market for thallium because of increased military requirements and expanded peacetime uses, the Salt Lake Station of the Bureau of Mines surveyed the occurrence of thallium in ores, concentrates, and smelter products from all parts of the nation and found the most promising source was certain smelter products of the American Smelting & Refining Co. plant, Murray, Utah. Much of the thallium was being lost in marketed arsenic products; therefore, this investigation was undertaken to develop methods for recovering the thallium.

Jan 1, 1952

By John A. Breslin

Size distributions and concentrations of particulates emitted from diesel engine exhausts were measured with cascade impactors. Samples were taken from the exhaust of two types of engines using three types of fuel and operating under five different engine speed and load conditions. The measured mass median diameters of the diesel particulates were typically about 0.3 um. There was no significant difference in mass median diameter between engines or fuels and only a slight dependence on operating mode. Concentration measurements ranged from 14.2 to 250.9 mg/cu m, and calculated mass outputs, from 52 to 3,443 mg/min. Significant differences in mass output were found between engines, fuels, and especially between different operating modes. The quantity of clean dilution air that would be required to reduce the particulate mass concentration below the 2.0 mg/cu m respirable dust standard for coal mines was greater than the dilution air required to meet the standards for noxious gases for both engines tested.

Jan 1, 1976

By F. P. Haver

The Bureau of Mines has investigated the electrochemical reduction of lead chloride as a method for producing lead without the pollution problems associated with smelting. It was determined that high-purity metal (>99.9 pct Pb) could be obtained, using PbC12 prepared by ferric chloride leaching of galena concentrate: PbS + 2FeCl3?PbCl2 + 2FeC12 + S°. Optimum results in small-scale electrolytic tests were achieved with a bath consisting of 40 to 70 wt-pct PbCl2 dissolved in KC1-LiCl eutectic, an operating temperature of 450° C, a current density of 2.5 amp/in2, and an electrode spacing of 0.5 inch. In large-scale tests made to develop a cell design for commercial application, the optimum electrode arrangement proved to be a bipolar configuration with horizontal plates. This gave a current efficiency of 86 pct with an energy requirement of 0.52 kwhr/lb lead. To determine the effect of impurity buildup in the bath, 1,200 lb of PbC12 prepared by ferric chloride leaching of galena concentrate was electrolyzed over a period of 2 months. Little deterioration of the metal quality occurred in that time; all of the lead produced had a purity equal to or better than corroding grade (>99.94 pct Pb).

Jan 1, 1976

By X. C. Shi

Bacterial mutagenicity and mammalian cell chromosomal and DNA damage in vitro assays were performed on a diesel exhaust particulate material (DPM) standard in two preparations: as an organic solvent extract, and as an aqueous dispersion in a simulated pulmonary surfactant. U.S. National Institute for Standards and Technology DPM SRM 2975 expressed mutagenic activity in the Salmonella reversion assay, and for in vitro genotoxicity to mammalian cells as micronucleus induction and as DNA damage in both preparations: as an acetone extract of the DPM mixed into dimethylsulfoxide, and as a mixture of whole DPM in a dispersion of dipalmitoyl phosphatidyl choline. Dispersion in surfactant was used to model the conditioning of DPM depositing on the deep respiratory airways of the lung. DPM solid residue after acetone extraction was inactive when assayed as a surfactant dispersion in the micronucleus induction assay, as was surfactant dispersion of a respirable particulate carbon black. In general, a given mass of the DPM in surfactant dispersion expressed greater activity than the solvent extract of an equal mass of DPM.

Jan 1, 2009

By George S. Rice

There have appeared, from time to time, comparisons of various features of coal mining practice in the United States and Great Britain. A recent, article, appearing in a British journal, points out that the American miner produces 3 1/2 times as much coal per shift as the miner, at one-half the cost, and proceeds to explain the natural industrial, and engineering causes which lead to this result. Amon« he reasons advanced. is that the American coal miner enjoys the advantage of more easily worked seams of coal, due to the fact that the coal mining industry in the United States is of more recent date than in Great Britain. The latter qualification is not correct, because where these advantages exist, they will persist. The coal beds of the United States are not buried deeply, except in the remote parts of the country, as in the Uinta Basin of Utah. The article referred to states that many of our miners are still employed on out seams reached by "adits", (which we term entries), or by vertical shafts of moderate depth. It is probable in fact that the great bulk of the coal of the United States is taken out from a depth of less than 400 feet.

Mar 1, 1920

By Erik Bengtsson

Phenol was discovered in coal tar by Runge (1)1/ in 1834 and was isolated (2) in 1841 as pure phenol by distilling the tar, extracting with caustic soda, acidifying the extract, and fractionating the tar acids. Later, o-cresol was isolated (3) through careful fractional distillation of the tar-acid mixture. The m-and p-cresols distilled within a boiling range of about 1.50 c. and had to be separated by other means. Raschig (4) fractionated the tar-acid mixture to obtain pure o-cresol, sulfonated the mixture of m-and p-cresols, and treated the cresol-sulfonic acids with superheated steam at 1200 to 1300 c. to hydrolyze the m-cresol sulfonic acid, the p-isomer was not affected at that temperature. He also attempted to make use of the different crystallizabilities of the m-and p-cresol sulfonic acids (5). When treated with sodium bisulfate and sodium pyro-sulfate at 100° to 110° C. or with sulfuric acid (90/0) at 20° C., only the m-cresol was sulfonated (6). Hoffman-La Roche (7) treated the meta-para mixture with concentrated sulfuric acid at 40° to 100° C., when m-cresol and part of the p-cresol was sulfonated, and precipitated the m-cresol sulfonic add by diluting with water. The same sort of separation may be carried out by means of 80 percent sulfuric acid at 35° C. and 35 mm pressure (8).

Jan 1, 1950

By R. B. Tippin

The heavy liquid separation (HLS) process was investigated by the Bureau of Mines to develop a means of concentrating minerals from natural ores, Various spodumene ores were tested in a 0.4-inch diameter cyclone using pure tetrabromoethane (TBE) as the heavy liquid. Studies were initiated to examine the influence of (1) pulp density (2) feed grade, (3) cyclone pressure, (4) cyclone apex opening size) (5) cyclone vortex finder opening sand (6) mineral particle size on the separation efficiency. Each of these factors was found to affect the heavy liquid separation in some degree; the mineral particle size exhibited the greatest effect and the ore feed grade the least. Conditions necessary to yield an 85 percent spodumene concentrate with an 85 percent recovery were determined to be: 70 psig pressure, 10 percent solids, 0.08-inch apex opening, 0.11-inch vortex finder opening and a minimum amount of minus 200-mesh fines in the feed. Operation of multiple cyclones in series resulted in spodumene concentrates assaying over 90 percent and indicated mineral recoveries exceed-in 90 percent.

Jan 1, 1967

By T. F. Anstett

The Bureau of Mines evaluated the potential availability of chrysotile, amosite, and crocidolite asbestos from 42 properties in market economy countries. This resulted in the development of tonnage-cost relationships indicating the quantity of grades 3 through 7 asbestos at various average total costs of production at 0% and 15% rates of return on invested capital. The availability of grades 2 and 8 was also evaluated, but since each is produced at only one property, no analytical results were given. Total demonstrated recoverable chrysotile fiber potentially available of grades 3 through 7 from the 42 properties evaluated follow: 1.59 million t, 21.00 million t, 16.74 million t, 15.54 million t, and 19.27 million t, respectively. The total amount of crocidolite is 1.69 million t. Owing to the good potential for discovery and development of new deposits, long- term availability of fiber of all three types is not in jeopardy. However, many of the crocidolite properties evaluated in the northern Cape crocidolite field of South Africa have relatively small demonstrated resources, and new deposits will have to be exploited by the late 1990's to sustain projected levels of production.

Jan 1, 1985

By K. A. Fowler, L. W. Higley

Steels with an alloying addition of depleted uranium were studied to develop successful melting , casting , and fabricating methods ; to obtain data on mechanical properties ; and to determine the effects of this alloying element . Uranium in amounts up to 1.5 percent was added to steel - base compositions containing approximately 0.5 percent carbon , 2 percent nickel , 0.25 to 2.0 percent silicon , and 0.75 percent manganese in both vacuum- melted and air -melted heats . Radiation levels were monitored for all operations . Bureau of Mines research at the Rolla Metallurgy Research Center showed that uranium additions did not increase tensile strength ; that hot - shortness occurred during forging above 1,090 ° C because of the presence of a low melting point constituent of a eutectic type ; and although a measurable amount of radioactive contamination resulted from processing , the quantity was never large enough to require the work area to be identified as a radiation area .

Jan 1, 1964

By J. A. Sutton

In connection with, a stream-pollution-research project, a colorimetric method was developed for concentrations of 1 to 30 p.p.m, of pine oil in water. The method depends on the stable bluish-green color produced when pine oil is reacted with vanillin-hydrochloric acid reagent at 60° C. for 25 minutes. The colorimetric reaction actually determines alphaterpineol, the principal component in pine oil. Some waters may require a special preparation in which ion-exchange resins are used to remove interference. ACKNOWLEDGEMENTS The author wishes to express his appreciation to A. A. Berk, chief of the Industrial Water Branch, Bureau of Mines, for helpful advice and encouragement during the progress of this work and to B. P. Martinez, chief of the Stream Pollution Research Section, for assistance with the manuscript. Thanks are also due to W. D. Bishop of the Hercules Powder Co., Wilmington, Del., for supplying the principal components of pine oil.

Jan 1, 1953

By Mulligan John J.

The Bureau of Mines investigated lode tin deposits on Potato Mountain, Seward Peninsula, Alaska. Tin was found to occur as cassiterite associated with quartz, tourmaline, pyrite, arsenopyrite, and earthy clays, but the deposits lack the varied accessory minerals commonly found in tin districts. The tin-bearing deposits are in metasediments along minor breaks and bedding planes but not in the crushed earthy filling of major faults. Cassiterite and sulfides occur with quartz in veins, both with and without earthy clays, and disseminated through tourmalinized wall rocks. The deposits are characterized by irregular segregations containing 1 to 10 percent tin within zones averaging not over 0.25 percent tin. The largest segregation exposed is on the summit of a low hill on the east-central slopes of Little Potato Mountain; most of the outcroppings are in an area trending east to west, roughly 10 to 30 feet wide and 300 feet long. Sample values ranged as high as 12 percent tin, but the average grade may be about 1 percent tin. The extreme irregularity of both grade and composition precludes a more exact determination. Similar concentrations are scattered for over 1,000 feet to the west and north, but these are smaller and lower in grade. Elsewhere on Potato Mountain, generally similar deposits occur as clusters of veinlets at widely separated points in the metasedimentary walls of major faults.

Jan 1, 1965

Greater mining productivity requires a more efficient cutting process. The cutting force available from today?s mining machines has been optimized with respect to machine size and weight. Researchers have shown that when employing water-jet-assisted cutting, bit forces and drum torques can be reduced significantly, which may allow mining machines to become lighter and more efficient. The Bureau of Mines has initiated a program to develop a water- jet-assisted rotary cutting system using the conventional bit assisted by a directed water jet operating at moderate pressures (3,000 to 10,000 psi). This water-jet-assisted cutting system has the potential to improve cutting efficiency without increasing machine horsepower or water usage (beyond what is presently used for dust control) or requiring fundamental changes in mining practice. IR addition to improvements in productivity, other anticipated benefits of water-jet cutting include reduced generation of respirable dust, elimination of frictional ignitions, increased bit life, reduced fines, and fewer machine vibrations. The papers presented at this open industry meeting discuss the development of water-jet-assisted cutting technology and future application of this technology to a variety of mining techniques including roof drilling and longwall mining.

Jan 1, 1985