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By A. W. Decora

Gas-liquid chromatography has been applied to separating basic nitrogen compounds, such as pyridines and amines. Close-boiling compounds have been separated by exploiting structural and polarity differences, using selective liquid substrates dispersed on specially prepared solid supports. Development of these special supports was necessary in order to obtain symmetric peaks for basic nitrogen compounds; solution of this problem was important in applying gas-liquid chromatography to the analysis of basic nitrogen compounds found in shale oil. Attempts to analyze shale-oil tar bases by conventional gas-liquid chromatographic techniques, using Chromosorb4/ or Celite 545 as the support for a nonpolar liquid substrate, resulted in asymmetric peaks. These asymmetries were caused by adsorption of sample vapors on the solid support. Symmetric peaks were obtained when strongly polar liquid substrates were used on either Chromosorb or Celite. However, a solid support giving symmetric peaks only with strong polar substrates restricts the choice of substrate, and frequently, desired separations cannot be achieved.

Jan 1, 1961

By Joseph Sabatini

This report, covering the period January through December 1975, contains abstracts of articles concerning all phases of cost engineering and economics for chemicals processing, raining, and other mineral industries. The abstracts are collected from the following sources: 1. Chemical Engineering 2. Chemical Engineering Progress 3. Chemtech 4. Coal Arse 5. Coal Mining and Processing 6. Combustion 7. Drilling 8. Electrical World 9. Engineering and Mining Journal

Jan 1, 1976

By P. L. Woolf, N. Bernstein, M. M. Fine

Continuous experimentation utilizing a 3- by 36 - foot rotary kiln was conducted to demonstrate the feasibility of simultaneous induration and reduction of magnetic taconite concentrate . Lignite , or lignite - anthracite mixtures , and green magnetite pellets (64.2 percent Fe , dry basis ) were heated in a rotary kiln to about 2,100 ° F. After separation from excess reductant , the product pellets were found to be highly reduced and acceptably hard . A total of 140 tons of prereduced pellets with an average Fe content of 79.0 percent was produced at Minneapolis and smelted in the Bureau's experimental blast furnace at Bruceton , Pa . Two additional supplies of prereduced pellets were obtained from The Steel Company of Canada , Ltd. , Hamilton , Ontario , which contained 83.8 and 91.3 percent Fe , respectively . Smelting of prereduced pellets was compared with that of unreduced pellets obtained from The Hilton Mines , Shawville , Quebec , and from the Erie Mining Co. , Hoyt Lakes , Minn . Blast furnace tests established that a substantial decrease in coke rates and higher production result from the use of prereduced pellets .

Jan 1, 1964

By J. D. Ramsdell

The object of this investigation by the Federal Bureau of Mines was to evaluate the workability, recrystallization characteristics, and mechanical and physical properties of high-purity electrorefined vanadium. The low level of interstitially soluble elements in electrorefined vanadium results in a soft ductile metal which responds readily to cold working by rolling, swaging, and press-forging. Hardness, strength, and resistivity increased with an increase in impurity content, but thermal expansion was independent of impurity content. The work-hardening of vanadium occurs rapidly. Most of the hardness increase occurs in the first 15 pct. of reduction in area. When vanadium is annealed, its hardness increases to a maximum when the annealing temperature is between 200° to 400° C. A sharp decrease in hardness develops as the annealing temperature is increased. An anomaly in the hardness versus annealing temperature curve is present in the 600° to 800° C. range, while all evidence of cold-work is removed at annealing temperatures above 900° C.

Jan 1, 1961

By H. E. Powell

Basic data were recorded on the decompositions that take place during thermal decomposition of siderite (FeC03). Both the naturally occurring and a synthetically prepared mineral were studied by differential thermal, thermo-gravimetric, X-ray-diffraction, and chemical (including gas) analyses. Thermal decomposition was studied in the media of dry air, moist air, dry carbon dioxide, dry helium, and dry carbon monoxide and at atmospheric and at reduced pressures. Results showed the thermal decomposition of FeC03 to be an extremely complex process, dependent on environmental factors and side reactions that cannot now be completely controlled. Therefore, full understanding of the reaction involved must depend on additional research with advanced evaluation techniques.

Jan 1, 1965

By E. G. King

Thermodynamic calculations involving the oxides of tungsten and molybdenum have been hampered by lack of accurate entropies and high temperature heat contents. This paper presents work by the Federal Bureau of Mines on new low-temperature heat-capacity data leading to the evaluation of the 298.15° K. entropies of tungsten dioxide and tungsten trioxide, as well as high-temperature heat contents (above 298.15° K.) of molybdenum dioxide, molybdenum tri-oxide, tungsten dioxide, and tungsten trioxide. Included are heats of fusion of the two trioxides. The heats of formation at 298.15° K. of these four oxides are tabulated as measured by Mah4 5/ of this laboratory. Included also are the 298.15° K. entropy of Mo02 measured by Kin 6/ of this laboratory, and that for Mo03 according to Kelley and King.7/ These basic data provide a consistent compilation from which to perform accurate thermodynamic calculations involving these compounds. No previous low-temperature- heat-capacity measurements have been reported for tungsten dioxide. Seltz, Dunkerley, and DeWitt8/ measured the low-temperature heat capacity of tungsten trioxide. The only previously-reported high-temperature heat-content measurements for any of the oxides were conducted by Cosgrove and Snyder,9/ who measured molybdenum trioxide to 1,300° K.

Jan 1, 1960

By D. Bienstock, R. C. Kurtzrock, E. R. Bauer, J. H. Field

To remove hydrocarbons and carbon monoxide in automotive exhaust by oxidation , a catalyst of 4.2 percent Uз Og , 1.7 percent Cr₂ 0 , and 1.7 percent CuO supported on 1 /8 - inch y- alumina spheres was tested in a reactor in place of the muffler of a 1 / 2 - ton truck . Tests were made with both nonleaded and leaded gasolines . With the engine at operating temperature , tests were made with the engine idling and with the vehicle cruising at 30 mph . Auxiliary air was added to maintain an oxygen concentration of 3 to 4 percent in the gas leaving the catalytic reactor . The vehicle was operated for 83 hours (about 60 percent of the time with the engine idling ) and 525 miles with nonleaded gasoline . Conversions of 98 percent of the hydrocarbons and 100 percent of the carbon monoxide were achieved with the engine idling and with 7,000 ppm carbon atoms and 4- percent carbon monoxide in the feed to the reactor . Hydrocarbon conversions of 75 percent were obtained at cruising speeds of 30 mph with a feed of 1,700 ppm carbon atoms ; the carbon monoxide concentration was less than 0.3 percent in the feed and was unchanged in passage through the reactor . Identical activity was obtained initially in switching to a gasoline containing 1.9 ml tetraethyl lead (TEL) per gallon . However, there was a gradual loss in activity thereafter . Conversions in tests with the engine idling about 50 percent of the time , had decreased by 23 percent for the hydrocarbons and by 25 percent for the carbon monoxide from their initial values after 122 hours and 1,300 miles of operation with leaded gasoline . The levels of radioactive materials in the exhaust of the reactor and the radiation in the vehicle were negligible .

Jan 1, 1963

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

An investigation was conducted to determine the relationship between ASTM and Micum tumbler data and to develop equations that would enable the conversion of data from one test method for comparison with those determined by the other , and thereby facilitate the international exchange of data . Relative strengths of 18 commercially produced cokes were determined by ASTM and Micum tumblers and ASTM shatter test . Two of the samples were coke produced for foundry use , and two were produced in beehive ovens . The remaining 14 samples were produced for blast furnace consumption and had ASTM tumbler stabilities of 36 to 58. Statistical procedures were used to relate the three test methods and also to evaluate the effect of charge weights , top sizes of coke , and types of screens specified by the two standard tumbler procedures , square - hole wire mesh for the ASTM tumbler and punched round - hole for the Micum . A significant result was that the data obtained with like screens have a higher degree of correlation with a smaller standard deviation than data from the screens specified for each tumbler .

Jan 1, 1964

By A. E. Petersen

To reduce U.S. dependence on imports of titanium, the U.S. Bureau of Mines has investigated the recovery of titanium from perovskite (CaTi03). Domestic perovskite deposits represent a significant, but untapped, titanium resource. An acid sulfation method was developed that will extract about 97 pct of the titanium and the columbium and 70 to 90 pct of the rare-earth byproducts from perovskite concentrates. A flow-sheet for recovering titanium as pigment-grade titanium dioxide (Ti02) is discussed. Test work performed in developing each unit operation is described. The first three unit operations have been demonstrated using laboratory-scale continuous methods of operation: acid sulfation of perovskite concentrates, leaching sulfation residue to dissolve metal values, and precipitation of titanium oxysulfate monohydrate (TiOS04?HP) from the resulting leach flltrate. Batch testing of other unit operations was performed: TiOS04?H20 redissolution and iron reduction, precipitation of Ti02 by hydrolysis, and regenerating recoverable acid with rare-earth byproduct recovery. Cost evaluation results are provided, indicating that processing perovskite concentrates by acid sulfation may be an economically viable means of producing Ti02.

Jan 1, 2010

By John W. Sweeney

Shales and clays from Illinois were sampled, tested, and evaluated to determine feasibility of producing lightweight aggregate by rotary-kiln methods. Sampling procedures and the 1 ,,,y of the Pennsylvanian shale units are discussed. Chemical, X-ray spectrographic and X-ray petrographic analyses were run on the samples to determine if a correlation existed between chemical mineralogic composition and expansion. Preliminary expansion testing was conducted in a muffle furnace. Rotary-kiln tests were conducted in a 16- inch by 14-foot rotary kiln. The weight of the aggregate ranged from 27 to 59 pounds per cubic foot. Concrete cubes employing the aggregate were tested to determine the qualities of the concrete. Compressive strength of the concrete using the 7-bag of cement cement per cubic yard mix, after autoclave curing for 6 hours, ranged from 2,950 to 6,750 psi. No correlation was found between the chemical, X-ray spectrographic, and X-ray and petrographic analyses and expansion, Sixteen samples made suitable lightweight aggregates in the laboratory rotary kiln. The expansion temperature range of eight of the samples was extremely narrow, and difficulties would probably be encountered in processing these materials commercially.

Jan 1, 1965

By John S. Ball

Aniline points have been used to some extent for more than 20 years. to indicate the types of structures in hydrocarbons and thus to analyze mixtures of hydrocarbons . This type of analysis has been applied - principally to the low -boiling hydrocarbons found in the gasoline range . Although there is some disagreement as to their merits , both aniline point and diesel index (aniline point in degrees Fahrenheit times A.P.I. gravity at 60 ° F. divided by 100) are used rather extensively for evaluating ignition qualities of diesel fuels . In recent years aniline points have been employed in the study of lubricating - oil fractions . They also have been used to predict : the tendency of different oils to cause swelling of synthetic rubbers.5/ Recent standardization of the aniline - point determination by the American Society for Testing Materials has encouraged wider use of this test . Considerable data concerning , aniline points and critical solution temperatures in aniline have been accumulated in the course of a study of related subjects . Thesc data , together with some original results , are presented here in the hope that they will prove useful to other worker's in this field ...

Oct 1, 1943

By D. Harrington, W. J. Fene, H. B. Humphrey

In the fiscal years 1946 and 1947 the number of mine explosions decreased compared with the preceding years. However, the loss of life was so serious during the fiscal year 1947 the period when the Government administered bi- tuminous-coal and lignite mines that from April to June 1947 extraordinary measures were taken in mines then under Government possession to obtain com- pliance with provisions concerning rock dusting, ventilation, and blasting that had not been followed. The great loss of life in explosions during the fiscal year 1947 as compared with 1944, 1945, and 1946 is not easy to explain, but the necessity for maintaining adequate protection has been definitely demonstrated. Management, workers, and inspection agencies alike must keep the mines reasonably safe against explosions or allow them to lapse into a condition where chance is the principal protection against disaster. The at- tention given to protecting coal mines and the men employed in them against mine fires, following the disastrous fires in 1944 and 1945, has at least tem- porarily controlled this hazard loss of life from coal-mine fires was re- duced to 1 fatality in 1947. The number of fires was also less, and progress has been made in reducing the heavy losses in both life and property from un- derground coal-mine fires that occurred in the two years mentioned. Fatalities from mine explosions during the past 6 fiscal years, July 1942 to June 1947, totaled 674, and there were 149 explosions; during the preceding 6 years there were 655 fatalities in 132 explosions. The 6 fiscal years 1942- 47 cover the active period of Federal coal-mine inspection. During the fiscal year 1947, there were 154 fatalities from explosions compared with 58 during the fiscal year 1946, 64 in 1945, 94 in 1944, 152 in 1943, and 152 in 1942.

May 1, 1948

By Frank J. Wiebelt

Under a general program to extend the resources of mineral deposits, the Bureau of Mines examined the Quien Sabe antimony mine in October 1948. The preliminary evaluation demonstrated that a diamond-drill program was warranted co establish the tenor and persistence of the veins and permit an estimation of antimony reserves. The Bureau of Mines conducted a diamond-drilling program on the property from December 1949 to May 1950. Ten holes aggregating 2,483 feet were drilled. Nine of the holes encountered antimony-bearing vein material.

Jan 1, 1956

By Gilbert M. Farrior

Tests of resistance to molten metals , to oxidation at elevated temperatures , and to various chemical reagents were made for a series of compositions in the TiB₂ - CrB₂ subsystem . In reaction with molten metals , there was no noticeable difference in reaction of the various compositions in the ( Ti , Cr ) B₂ series . The oxidation tests were ( 1 ) a rising - temperature test in which the specimen temperature was increased 4° per minute to 1,200 ° C and ( 2 ) a constanttemperature test in which the specimen temperature was held constant at 1,000 ° C. Compositions near Tio.6 Cro.4 B2 had the best oxidation resistance . Ti。.6 The chromium- rich alloys showed marked superiority to the titanium- rich alloys in resistance to corrosion by the chemical agents investigated . The chemical reagents used were sulfuric , nitric , and hydrochloric acids and sodium hydroxide of different concentrations .

Jan 1, 1964

By A. C. Burr

This progress report covers the period from January 1949 to the end of the fiscal year, June 30, 1950. Three runs were successfully completed, and one run was terminated as the result of failure of a cast reaction tube. Including the abbreviated run, the gasifier was operated for 1,915 hours, during which some 428 tons of natural and steam- dried lignite was partly gasified In producing 20 million cubic feet of gas. Gas-production rates varied from 7.8 to 16.4 thousand cubic feet per hour, the latter being the highest production rate yet reached; hydrogen-carbon monoxide ratios of the product gas varied from 1.85, the lowest ratio yet produced, to 6.5; and heat-transfer rates through the heated wall of the outer tube varied from 2,100 to 4,400 B.t.u. per square foot an hour. The general objective of the project is to establish the technology and economy of the gasification of lignite in an externally heated, metal, annular retort. Specific objectives include determination of the useful life of the metal retort tube, which is a continuing problem, and special objectives that were established for each run as part of the systematic investigation of the basic variables of the gasification process. For runs 10 and 11 the special objective was the influence of the lignite feed rate on gasification; for run 12, a comparison of dried and natural lignite, and the production of gas having a hydrogen-carbon monoxide ratio less than 2; and for run 13, the influence of a gradually increasing steam rate with steam admitted to either the upper or lower reaction zones. In addition, during each run the sulfur distribution and concentration in the product gas and char were investigated. Experimental results obtained using the lignite feed rate as the variable indicated that the gas yield per ton of natural lignite varied inversely with the feed rate. Comparison of the gasification of natural and steam-dried Dakota Star lignite indicated that the dried lignite was a superior gasification material because: 1. The hourly gas production was higher at normal combustion space temperatures under nearly equal experimental conditions. 2. On the moisture- and ash-free basis, a considerably higher feed rate could be maintained at a relatively high percentage of carbon gasified. 3. At nearly equal moisture- and ash-free feed rates, the specific gas yield was higher. The location of steam admission was found to be important because the gas yield per ton of natural lignite was higher when at least a portion of' the process steam was admitted to the upper reaction zone. Heat balances showed the potential heat in the gas and char to be 71.8 to 83.6 percent of the total heat input. The sulfur concentration in the product gas was low, being in the range of 35 to 140 grains per 100 cu. ft., of which 1.5 to 2.3 grains was organic sulfur. Careful measurements and inspection of the 310-alloy rolled plate tube following runs 11, 12, and 13 showed no excessive corrosion; however, some radial deformation had occurred indicating that deformation or creep might be the limiting factor in the life of the tube.

Jan 1, 1953

By V. F. Parry

[Approximately 7-1/2 million tons of subbituminous coals are mined annually in Colorado, Wyoming, and Montana, of which 50 percent probably reaches domestic consumers. The moisture of these subbituminous coals is high, averaging about 25 percent when they are mined. The coals are non-caking end stack to a variable degree when exposed to normal atmospheric conditions. They are good domestic fuels, are considered to be smokeless in most furnaces, and have been used for many years in hand-fired domestic furnaces in which the practice is to employ large lutes for efficient combustion.]

Jan 1, 1941

By Paul Hatmaker

Lime was a highly useful commodity thousands of years before the simple chemistry of its manufacturing process was known. The employment of lime for agriculture, building, and even certain essentially chemical purposes is so old that its origin is among the unrecorded details of man's first ventures into the manufacture and use of prepared substances. Lime is a most versatile material and consequently has come to be widely utilized in modern civilization. Immediately before the depression of the early 1930's the annual production of lime in the United States was more than 4 million tons, valued at 33 to 42 million dollars. This output was sold to many industries, so many that mere enumeration becomes tedious. In addition to agricultural and building lime the sales statistics compiled annually by the Bureau of Mines include lime sold to the steel and other metallurgical industries as refractory and fluxing material, as well as that used by paper mills, glass works, tanneries, and water-treatment plants. These major uses normally consume about 86 percent of the domestic sales. The remaining 14 percent includes lime sold for use in the manufacture of alcohol, alkalies, bleaches, calcium acetate, calcium carbide, coke gas and byproducts, glue, insecticides, oils and fats, paints, and rubber, in the refining of salt, in the manufacture of sand-lime and slag brick, in the disposal of sewage and garbage, in the manufacture of silica brick, in the refining of sugar, in the textile industries, and in wood distillation. Many other uses are also known for which complete sales data are not available.

Jan 1, 1934

By A. L. Service, C. C. Popoff

Phosphate deposits in Montana , Idaho , Wyoming , and Utah are important factors in the mineral , agricultural , and industrial economy in the western part of the Nation . This report presents background information , including geology , mining , beneficiation , processing , resources , and economics , assembled to provide a comprehensive introduction to a series of four area reports . About 20 percent of the Nation's phosphate is produced from the Western field where there were 6 surface and 9 underground mines in operation in 1963 . This region also has an estimated 58 percent of the Nation's phosphate reserves , and continuing development is assured by these abundant resources and an increasing demand for phosphate products . Long range forecasts indicate that the United States will continue to use increasing amounts of both agricultural and industrial phosphate products . Beneficiation has become an important part of the phosphate processing industry , and two flotation plants and several washing plants were in operation in 1963. Recent studies by the Bureau of Mines Metallurgy Research Center , Albany , Oreg . , have been directed toward developing flotation processes applicable to treatment of marginal phosphate rock . Other Bureau of Mines research is being directed toward improved methods of ore recovery , ground control , and mining .

Jan 1, 1964

By Lloyd H. Banning

Crucible-smelting tests at the Northwest. Electrodevelopment Laboratory and a pilot-plant test on electric smelting of western phosphate rock for the Westvaco Chlorine Products by the Tennessee Valley Authority indicated that the small vanadium content of the rock is concentrated in the ferrophosphorus by-product of Phosphorus smelting. This research is concerned' mainly with recovering vanadium and phosphorus froth the ferrophosphorus produced from western phosphate rock. Exploratory tests were made of several methods of treating vanadiferous ferrophosphorus. Attempts to separate vanadium as a carbide dross by saturating molten ferrophosphorus with carbon were unsuccessful. Volatilization of phosphorus from ferrophosphorus was accomplished to some extent, both with and without addition of sulfur in several forms, but elimination of phosphorus was not complete. Brief testing in a small experimental converter on oxidation of vanadium and phosphorus; into a slag by blowing with air showed promise. A method that comprised fusing vanadiferous ferrophosphorus mixed with soda ash under oxidizing conditions gave encouraging results and was tested beyond the preliminary stage. A slag product of the fusion contained most of the phosphorus and vanadium as water-soluble sodium phosphate and. virtually water-insoluble sodium vanadate. After leaching the sodium phosphate froth the slag, the leach residue was reroasted with soda ash and salt. This roasted product was leached again with water to extract the vanadium.

Jan 1, 1951

By Oliver C. Fursman, Lloyd H. Banning

This research was undertaken to determine the feasibility of producing steel from hydrogen - reduced , pyrophoric iron powder . Before steelmaking tests were begun , investigations were made to develop procedures for handling the pyrophoric powder safely , and melting tests were made in a single - phase , electric - arc furnace to determine inert gas requirements for preventing powder oxidation . Steelmaking tests were conducted in a conventional electric - arc furnace , usually by a two - slag basic procedure . Results of the research indicated that ( 1 ) pyrophoric powder can be handled safely and can be prevented from oxidizing excessively during charging and melting in electric - arc steelmaking furnaces ; ( 2 ) little , if any , more electrical energy is required for melting Cerro Bolivar iron powder per unit of contained iron than is required for melting heavy melting scrap ; ( 3 ) high - quality steel can be produced readily from high- grade iron powder , having recoveries up to 95 percent of the total iron ; ( 4 ) steel can be produced from simulated titaniferous , chromiferous , and manganiferous iron powders ; and ( 5 ) the electrical energy required for melting increases with increase in the proportion of slag - forming constituents in the furnace charge .

Jan 1, 1964