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By J. W. Horne, W. B. Shirey

"INTRODUCTION The United States Bureau of Mines in cooperation with the State of Colorado at the University of Colorado has conducted experiments to determine the amount and composition of the noncondensable gases evolved when crude shale oil is distilled under pressure.Hydrogen sulphide is one of the components found in the complex mixture of gases produced by the distillation of shale oil under pressure. This paper deals with the apparatus and method used in determining the amount of hydrogen sulphide evolved in the laboratory experimental cracking stills.The study required a complete extraction of all the hydrogen sulphide from the gas stream after it left the water-cooled distillate condensers and before the as stream entered the charcoal absorber for removing the light naphtha. In devising the method it was necessary to take into account a constant variation of velocity, pressure, and percentage of sulphide in the total gas stream coming from the still.Ordinarily, the quantitative determination of hydrogen sulphide in Gas is made by analyzing small samples taken at regular intervals. This estimation can be accomplished by use of the Bunte gas burette as modified by Tutriler,4 or by a similar method. In the industries where the flow of as is constant end of uniform composition, this practice is sufficiently accurate for plant control. For experimental work where many variables have to be taken into consideration, as in the case at hand, these methods are not applicable."

Oct 1, 1931

By J. P. Hansen

In order to help assure an adequate domestic supply of minerals essential to the Nation's economy and and security by developing more efficient minerals extraction technologies, the Bureau of Mines Tuscaloosa Research Center examined the application of autogenous microgrinding to calcium carbonate minerals. Treatment of minus 8-mesh Alabama marble resulted in a product 80 pct minus 5 micrometers (µm) at a power consumption of 70 to 80 kwhr/ton, This study shows that coarse particles of calcium carbonate minerals are effective as the grinding media for the autogenous attrition grinding of these minerals. The minus 8- plus 30-mesh fraction is an effective grinding medium (sand) for particles smaller than 30 mesh. A 40-pct-solids slurry and a sand: marble ratio of 2.5 appeared to be near optimum. For residence times above 13 minutes, products were greater than 80 pet minus 5 µm and greater than 54 pct minus 2 µm. Power consumption was uniformly low, ranging from 50 to 100 kwhr/ton of product depending upon the feed rate. One marble sample from Georgia was shown to be the most persistent grinding medium, with losses of less than half those of the other materials tested.

Jan 1, 1980

By R. E. Perry

To develop new or improved flotation methods for beneficiating low-grade red iron ores, the Bureau made many bench scale and continuous anionic flotation tests on ferruginous sandstones and calcareous iron ores from the north-eastern part of the Birmingham, Ala., iron district. The ores contained about 21 to 36 percent iron, a to 11 percent lime, and 22 to 64 percent silica. Production of iron concentrates containing 48 to 52 percent iron was technically feasible in batch tests, and the iron recoveries ranged from 85 to 92 percent. In continuous tests 49 to 51 percent iron products were obtained with 80 to 90 percent recovery.

Jan 1, 1962

By D. J. Bauer

The Bureau of Mines demonstrated the feasibility of fractionating lanthanide nitrates with a tertiary amine on lanthanum-cerium and thulium-ytterbium pairs. Optimum values were determined for pH, phase concentration, and percent chelation of metal ions in the aqueous phase. Percent extraction is markedly dependent on the concentration of lithium nitrate in the aqueous phase. Selective masking of the heavier element in each extraction system with DTPA or EDTA aqueous-phase chelating agents resulted in lanthanum-cerium separation factors of 8.5 and thulium-ytterbium separation factors of 3.4.

Jan 1, 1966

By J. M. Stuve

Standard heats of formation (AH°p) of YbCl3 (c) and TmCl3 (c) were measured by solution calorimetry. Heat of solution data are given for ytterbium and thulium metals and corresponding anhydrous trichlorides in 4.360 molal hydrochloric acid. The derived standard heats of formation of YbCl3 (c) and TmCl3 (c) were -229,370 ±720 and -235,820 ±400 cal/mole, respectively, at 298.15° K. The resulting heats of formation for YbC13 and TmCl3 are about 1 kcal and 6.3 kcal more negative than previously published values.

Jan 1, 1967

By M. Shabbir

A study was made to determine the optimum conditions for precipitation of uranium from mill solutions using hydrogen peroxide. Precipitation tests were made on both synthetic and actual mill solutions. Parameters studied included amount of hydrogen peroxide, initial pH, reaction pH, time, and temperature. Also investigated was the effect of varied amounts of vanadium, molybdenum, and sulfate in the test solution on uranium precipitation and product quality. The optimum conditions for complete precipitation and high product quality were (1) the use of 150 percent of the stoichiometric requirement of hydrogen peroxide, (2) initial pH of 1.0, (3) reaction pH between 3.4 and 5.0, (4) 4 hours reaction time, and (5) ambient reaction temperature. The excess hydrogen peroxide requirement is partially dependent on the amount of impurities present in the feed solution. The hydrogen peroxide process appeared applicable to treatment of the several mill eluate and strip solutions tested. The experimental studies also indicated that the hydrogen peroxide technique gives substantially better product quality than that produced by ammonia precipitation.

Jan 1, 1974

By G. R. Fitterer

In the manufacture of steel by any process the refining period involves the partial elimination of the metalloids carbon, manganese, phosphorus, and silicon, by virtue of their reactions with ferrous oxide. At the end of this refining stage the metal consists chiefly of iron in which small amounts of these materials are dissolved. Unless some deoxidizer is added to the steel at this time, the reaction between carbon and ferrous oxide will continue with such force that it is impossible to form sound steel in the ingot molds. Instead, the product will exhibit a marked porosity due to the formation and trapping of carbon monoxide-the product of the reaction mentioned. However, if deoxidizers are added, steel may be obtained which is dense and free from gas bubbles. At the same time the deoxidation products will remain in the steel as impurities. For example, silicon additions form SiO2 or combinations of SiO2 and FeO. Additions of manganese form deoxidation products consisting of various proportions of MnO and FeO. It is also quite obvious that simultaneous additions of manganese and silicon will form oxide combinations either in the binary system MnO-SiO2 or in the ternary system FeO-MnO-SiO2. Work at the Pittsburgh Experiment Station of the United States Bureau of Mines, in cooperation with the Carnegie Institute of Technology and the Metallurgical Advisory Board, involved the study of such deoxidizing reactions and their products. In this connection considerable information is necessary concerning FeO, MnO, SiO2, and Al2O3, and their various combinations. Some of the most needed data are the melting points of all of these materials. At the outset of this work ordinary methods of melting point determinations were found to be inadequate for various reasons, and the procedure finally selected involved the use of the micropyrometer with occasional corroboration by quenching methods. The reasons for this selection, together with a description of the apparatus, are given in the following pages.

Jan 1, 1932

By Thomas C. Ruhe

The Pittsburgh Research Laboratory of NIOSH conducted research to determine the safe operating conditions for using recycled (used) lubricating oil from mining equipment as a partial replacement for diesel fuel to make ANFO-type blasting agents. The use of recycled oil (RO) conserves energy, reduces oil imports, and reduces mining costs. Since RO has a variable composition, there was concern that the additives/impurities it contains may cause ANFO made with RO to be unstable (as compared to regular ANFO) at high summer ambient storage temperatures. Reactivity of RO with zinc was also a concern. Thermal stability tests were conducted to help quantify and resolve these issues. ANFO mixtures (0.66 lb/300 g) were put into sample containers made of steel, stainless steel, and galvanized (zinc coated) steel pipe fittings, which were heated in isothermal ovens. The experimental parameters were temperature settings of 140° F (60° C) and 176° F (80° C), four sample container (pipe fitting) metal combinations, and nominal heating periods of one and three days. The ANFO samples contained 6% each of the following twelve different oils/oil mixtures: No. 1 was diesel fuel, Nos. 2 thru 6 were five candidate oils (2 thru 5 were used oils and 6 was a new synthetic oil), No. 7 was 5% diesel fuel + 1 % graphite, and Nos. 8 thru 12 were 3% diesel fuel + 3% each of the five candidate oils. All samples showed no reactivity when heated at 140° F (60°C). All samples (except No. 7) reacted at 176° F (80° C) in a steel pipe with galvanized caps as follows: No. I reacted most, Nos. 8-12 reacted moderately, and Nos. 2-6 reacted least. All ANFO samples were tested and found not to be cap sensitive.

By Arden D. Fugate

This work was conducted to determine a feasible process for converting siliceous fluoride offgases to a commercially usable product. The offgases were generated by pyrohydrolytic defluorination of low-grade fluorspar in a gas-fired rotary kiln, and fluorine was collected as a hydrofluoric-fluosilicic acid. A silicon-free fluoride solution for further processing was then produced by neutralizing the acidic scrubber solution with anhydrous ammonia, silicon being separated as orthosilicic acid. Ninety to ninety-nine percent of the fluorine originally present remained in solution as ammonium fluoride. Silicon was also separated from synthetic fluosilicic acids, having F-to-Si weight ratios ranging from 3.50 to 14.3. The solutions below a ratio of 4.06, the F-to-Si ratio of H2SiF6, containing dissolved silicon were desiliconized as completely as those containing less than the stoichiometric quantity of silicon. An electrolytic-grade cryolite was recovered from the ammonium fluoride solution by reacting with either sodium aluminate or alumina trihydrate and sodium hydroxide. A product containing 97 to 100 percent of the fluorine, represented by Na3A1F6, was recovered, and 94 to 99 percent of the theoretical yield was realized.

Jan 1, 1963

By Arno C. Fieldner, J. W. Paul, WALTER A. SELVIG

Many mine samples of coal are analyzed each year in the laboratories of the Bureau of Mines. The analyses are made in connection with investigations relating to fuels belonging to or for the use of the United States Government, the causes of accidents in coal mines, the geologic relations of coal beds, and the quality and the value of the coal and lignite in the public lands. The systematic collection and analysis of such samples in connection with fuel investigations was begun in 1904 at the Government fuel-testing plant at the Louisiana Purchase Exposition. and was under the direction of the United States Geological Survey for six years. Descriptions of the coal samples collected between the beginning of this work, July 1, 1904, and the transfer of the fuel-testing and mine-accident investigations to the Bureau of Mines,July 1, 1910, were compiled and published in Bureau of Mines Bulletin 22.' Descriptions and analyses of samples collected during the fiscal years 1911 to 1913 were published in Bureau of Mines Bulletin 85.2 Descriptions and analyses of samples collected during the fiscal years 1913 to 1916 were published in Bureau of Mines Bulletin 123.3 The present bulletin presents analyses and descriptions of samples collected during the fiscal years 1916 to 1919. In order that the material in this bulletin may be used to supplement that presented in Bulletins 22, 85, and ,123, the same plan of geographical classi- fication has been followed, the analyses and descriptions of the samples being grouped in alphabetical order according to the State, county, and town near which the mines or prospects sampled are situated.

Jan 1, 1922

By J. B. Zink, M. J. Peterson

A semiquantitative spectrochemical method was developed and applied to the analysis of ash of U.S. coals . A low- temperature ashing procedure was used to minimize the loss of volatile elements . The analytical procedure provides for the estimation of 68 elements including major , minor , and trace constituents . Standards for the trace elements were prepared in a synthetic base mixture that approximates the average composition of U.S. coal ashes . Excitation was achieved with a d- c arc , spectra were recorded photographically , and interpretation was made by visual comparison of spectra of unknowns with spectra of graded standards series . Thirty- six trace elements were found in the analysis of 900 samples . Details of the procedure are presented , including sample and standards preparation , excitation and exposure conditions , spectral lines used , and approximate limits of detectability .

Jan 1, 1964

By F. E. Block

The reaction between calcined dolomite and ferrosilicon has been studies with the aim of developing a continuous process for magnesium production. Small-scale tests were made in vacuum retorts similar to those used in the vacuum retort process as developed by Pidgeon (1)2/ and operated during the period of World War II in several Government-owned plants. Factors investigated with respect to the silicon efficiency were the reaction temperature, reaction time, amount of excess dolomite in the charge, and effect of adding sodium silicate to the charge to serve as a binder. Additional laboratory tests were made to study the reaction at elevated temperature but at atmospheric pressure. Silicon efficiencies exceeding 80 percent were found to result when operating in the temperature range from 1,750° to 1,800° C. for periods of 20 to 30 minutes.

Jan 1, 1956

By A. J. Forney

A high-Btu gas was made at the Bruceton, Pa., laboratories of the Bureau of Mines to demonstrate the feasibility of using the gas as a nonpolluting fuel for automobiles. The pilot plants at Bruceton were revised to combine the processes of coal gasification, gas purification, and catalytic methanation in one overall system. Tests in the Bureau's test automobiles at Bartlesville, Okla., showed the Synthane gas was less polluting than natural gas.

Jan 1, 1972

By M. M. Wong, J. E. Klosterman

Scrap beryllium chips ( nominally 96 to 97 percent Be ) were electrore fined in a prototype cell with 408 lb of electrolyte composed of 52.4 mole - percent LiCl , 36.3 mole - percent KC1 , and 11.3 mole - percent BeCl2 . The cell temperature was 500 ° C. In a typical 10-3 /4 - hour deposition cycle , 0.415 pound of metal was produced ; the metal contained impurities in parts per million as follows : C , 700 ; 0 , 610 ; Al , 34 ; Ca , 32 ; Cu , 20 ; Fe , 25 ; Mg , 9 ; and Mn , 23 . Operation of the prototype cell for 2 years demonstrated that adapting the electrorefining process to an enlarged scale of operation presented few difficulties in mechanical functions , maintenance of optimum operating conditions , and control of product purity . After the spent anode feed was leached in a 5 - percent nitric acid solution and the fine - sized particles were removed , it was recycled in some tests . The metal produced was somewhat higher in impurities than metal from the fresh scrap chips .

Jan 1, 1964

By Russell R. Trengove

Bureau of Mines exploration at the property of the Tulare County Tungsten Mines was by core drilling from the surface from May 16, 1950, to July 13, 1950. The property is in the western foothills of the Sierra Nevada Range, 18 miles northeast of Lindsay, Calif. It has been in almost continuous production since 1942 and has produced 40,831 units of tungsten trioxide (W03) with a grade of approximately 67 percent. The work performed comprised a study of the geology, mapping the area, sampling the outcrops, and diamond drilling the area adjacent to the mine workings. Ten holes were drilled for a total of 1,824 feet. Ore reserves were found to be confined to tactite zones in a surface area approximately 250 by 400 feet and extending downward about 350 feet.

Jan 1, 1956

By Robert Lee Stahl

Comprehensive field tests were made in the Gas Hills, Wyo., to determine whether surface geophysical techniques could be used to detect and delineate faults in marginal uranium deposits. The tests were made on property owned by Federal American Partners, Gas Hills, Wyo., and included seismic refraction, self-potential, induced polarization, magnetometer, electrical resistivity, airborne infrared thermal scanning, and airborne photography. Of the several geophysical techniques tested in the field, horizontal resistivity profiling with electrode spacings in the range of 25 to 50 feet was most diagnostic of faults. The method is quick, cheap, accurate, and one that can be easily used by personnel employed by mining companies to detect and delineate faults.

Jan 1, 1973

By Maria I. De Rosa

The U.S. Bureau of Mines performed experiments to determine the hydrogen cyanide (HCN) concentrations and smoke particle characteristics during the combustion of flexible polyurethane foams and other nitrogen-containing materials, for the development of a test parameter. The experiments were conducted in an approximately 2O-L furnace at set furnace temperatures of 250° and 1,000° C for a 14-min duration, with an airflow through the furnace of 10 L/min. The variables studied as a function of time were the gaseous and aerosol HCN concentrations, the smoke particles average diameter (dg) and particle concentration (no), and the product of the smoke particle diameter and concentration (dgno). Carbon monoxide, carbon dioxide, and oxygen concentrations, sample mass weight loss, and furnace temperatures were also studied; analyses of nitrogen and cyanate content of the material were carried out. Results show that dgno correlates directly with the HCN concentrations, which depend on the nitrogen and cyanate contents of the material.

Jan 1, 2010

By John C. Machisak

The Nation's mining and quarrying industries have again met the annual challenge to their ingenuity--that of reducing disabling work injuries among their employees. The effectiveness of management in facing this problem and in meeting this responsibility from the results of the 1961 National Safety Competition. Three hundred ninety-three or 45.3 percent of the mines and quarries participating in the competition established a new record number of participants operating throughout the competition year without a disabling work injury. Another record established in the 1961 contest was the number of participants (868) enrolled in the competition. This annual safety competition was begun in 1925 and is conducted by the Bureau of Mines, U.S. Department of the Interior. It provides for six bronze Sentinels of safety trophies which are awarded each year to the winning participant in each group. Since its inception, the competition has exerted a strong influence in the field of safety promotion. The statistical record of its accomplishments over the years gives strong support to the theory that well-organized and well-administered safety programs are effective tools to be used to reduce the number of disabling work injuries. It stimulates and holds the interest of employees and management in accident prevention. Because of this, mines and quarries participating in the contest have a more favorable safety record than those operations not enrolled.

Jan 1, 1963

By John C. Machisak

The Nation's mining and quarrying industries have again met the annual challenge to their ingenuity--that of reducing disabling work injuries among their employees. The effectiveness of management in facing this problem and in meeting this responsibility is evident from the results of the 1961 National Safety Competition. Three hundred ninety-three or 45.3 percent of the mines and quarries participating in the competition established a new record number of participants operating throughout the competition year without a disabling work injury. Another record established in the 1961 contest was the number of participants (868) enrolled in the competition. This annual safety competition was begun in 1925 and is conducted by the Bureau of Mines, U.S. Department of the Interior. It provides for six bronze Sentinels of safety trophies which are awarded each year to the winning participant in each group. Since its inception, the competition has exerted a strong influence in the field of safety promotion. The statistical record of its accomplishments over the years gives strong support to the theory that well-organized and well- administered safety programs are effective tools to be used to reduce the number of disabling work injuries. It stimulates and holds the interest of employees and management in accident prevention. Because of this, mines and quarries participating in the contest have a more favorable safety record than those operations not enrolled.

Jan 1, 1963

By Sidney Katell

Tonnage oxygen plants are or can be made available in sizes ranging from 150 to 1,000 tons per day. Capital requirements are estimated from $5,400 to $14,700 per daily ton, depending upon size of plant, cycle employed, and purity and discharge pressure of the product. Similarly, operating costs before return on investment will range from $4.80 to $10 per ton. INTRODUCTION Several processes4 5/ that can be used to convert coal to synthetic liquid fuels, synthetic pipeline gas, or hydrogen require high-purity oxygen as one of the basic raw materials. Depending on the and product and its specific use, the oxygen required will be of 95 or 99.5 percent purity. The quantity required, in turn, depends on the process for which the oxygen will be used and the size of the processing plant and will range from 150 to 4,000 tons per day.

Jan 1, 1960