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By R. L. Hopkins, H. T. Rall

A continuous method has been developed for preparing thiolacetic acid . Acetic anhydride and hydrogen sulfide are passed concurrently over an amine ion- exchange resin , under 20 - psi pressure . The thiolacetic acid , a product of the reaction , is flashed continuously from the crude reaction mixture and is purified by fractional distillation . The yield of thiolacetic acid is in excess of 80 percent based on the acetic anhydride charged . INTRODUCTION In the synthesis of reference compounds needed in the identification of sulfur compounds in petroleum , thiolacetic acid has become an important reagent because of its use in the synthesis of thiols by addition to appropriate olefins : R - CH = CH₂ + CH3 - COSH R- CH2 - CH2 - S - COCH R - CH2 - CH₂ - SH + CH3COONa NaOH (1 ) The commonly used procedures for its preparation , as described by Clark and Hartman (1 )4 and by Ellingboe (2 ) , are based on the batchwise reaction of acetic anhydride with hydrogen sulfide :

Jan 1, 1964

By James L. Konchesky

Crushed coal, consisting of a wide range of sizes, was effectively blended by recycling it through a bin equipped with a particle distributor. Vertical blending was accomplished by simply recycling the coal; it was not significantly influenced by the horizontal blending that was achieved by the distributor. The method was effective, even though the coal was wet and possessed poor flowing characteristics. Recirculation appears capable of providing uniform blends of solids that can be more efficiently processed. Recirculation also appears useful, preceding packaging operations, to insure for blending of solids into specification products. Continuous measurement of the bulk density of the coal by a gamma ray meter proved to be an effective monitor of vertical blending effectiveness.

Jan 1, 1972

By H. C. Ko

The Bureau of Mines maintains an active program in thermochemistry to provide thermodynamic data for the advancement of mineral science and technology. As part of this effort, the standard enthalpy of formation at 298.15 K, ?Hf°, for 2CdO-CdSO4 was determined by HCI acid solution calorimetry to be -345.69 ±0.61 kcal/mol.

Jan 1, 1983

By R. Karl Zipf

A fatal explosion in a sealed area at the Sago Mine in 2006 prompted researchers and regulators in the United States to re-examine the requirements for explosion-resistant mine seals. Seals are used in underground coal mines to isolate abandoned mining areas from active workings. Prior to the Sago disaster, mining regulations required seals to withstand a 140 kPa explosion pressure. Recent research at the National Institute for Occupational Safety and Health (NIOSH)Pittsburgh Research Laboratory showed that pressures from explosions can far exceed this pressure. U.S. mining regulations now require much stronger seals. Current research focuses on understanding the science, engineering and management of sealed areas of coal mines. Scientific efforts seek understanding of how explosive methane-air mixtures accumulate using measurements and models of the sealed area atmosphere. Additional scientific efforts aim to understand the explosion pressures that can develop using a combination of numerical modeling and experiments. Engineering efforts aim to produce design guidelines for seals that can resist the new higher pressure design criteria. NIOSH researchers are also developing guidance for monitoring of sealed area atmospheres and inertization of potentially explosive gas mixtures within sealed areas. This paper seeks to encourage scientific discussion among international peers since preventing explosions within sealed areas is of interest to underground coal operators and regulators.

Jan 1, 2009

By Wilbur Duvall

For the past few years the Applied Physics Branch has been investigating, experimentally, the generation and propagation of strain waves in rock. The strain waves are produced by the detonation of a high-velocity explosive placed in a small cavity in the rock. Strain gages mounted in the solid rock surrounding the cavity record the strain pulses propagated away from the source. Numerous strain-wave pulses have been recorded in different rock types for charges of various sizes and at various distances from the charge. Analysis of these records has shown, among other things, that there is associated with the strain wave a characteristic pulse width. This pulse width is dependent on the rock type and the distance from the shot point to the gage, but is apparently independent of the charge size or cavity size. Recent published literature on the generation and propagation of seismic waves indicates that the characteristic frequency of an elastic wave generated by an explosion should be a function of the rock type and the size of the cavity created by the explosion. Also, internal friction in the rock would produce absorption of high-frequency components, which would cause continual change in the shape of the pulse propagated. As the experimental data did not verify the expected change in pulse shape with cavity size, a theoretical investigation of the vibrations associated with a spherical cavity in an elastic medium was undertaken.

Jan 1, 1950

By Richard L. Jenkins

Systematic sampling, in reconnaissance fashion, of the continental shelves of the United States to define favorable areas of offshore mineral deposits, is one of the long-range marine mineral; programs of the U.S. Department of the Interior. In mid-1966 the Department of the Interior launched its Heavy Metals Program to stimulate domestic output of gold which is in serious short supply. The program is jointly conducted by the Geological Survey and the Bureau of Mines.

Jan 1, 1968

By R. S. Dean

The principle of explosive crushing depends upon the fact that an expandable substance contained within the pores of a solid body will disrupt such a body upon expansion. Such expansion may be obtained by the detonation of an explosive or by the sudden release of pressure of a superheated liquid. That this principle of disruption may be applied to minerals rests on the fact that cracks, cleavage planes, and pores exist in all mineral to an extent hardly conceived possible heretofore. Crushing by this method takes advantage of force applied from within the mineral rather than from forces applied from without. The application of a force from within would appear to be more effective. A consideration of the possibilities of such a method for crushing led to some experimental work of a preliminary nature, the results of which are embodied in this paper. No systematic program was followed in the work and the results are, therefore, not final and far from complete. The success attained so far, with the mediocre apparatus available seems to warrant a preliminary report, with the expressed hope that the work may be carried on as well-outline program covering such phases as have been impossible to investigate at this time.

Jan 1, 1931

By Daniel Edelstein

The supply of arsenic trioxide in 1982 was adequate to meet domestic demand. Allocation of supply by major domestic and foreign producers that began in 1977 ended during the first quarter of 1982. Major demand was about evenly divided between industrial chemicals and agricultural chemicals. Domestic Data Coverage.-Commercial- grade arsenic trioxide and arsenic metal were produced by only one U.S. company. In order to prevent disclosure of proprietary data, arsenic production data have been withheld.

Jan 1, 1983

By M. M. Wong

A brief investigation was made to determine the feasibility of electro-refining beryllium in a KCI-LiCI-BeC12 bath. Thin, platelike crystals of beryllium metal were produced by electrolyzing technical-grade beryllium metal beads (about 94-percent purity) as the soluble anode. Operating cell conditions were: Temperatures of 450° to 600° C.; an inert atmosphere; bath compositions of (1) 38.1 mol. percent KC1, 54.8 mol. percent LiCl, and 7.1 mol. percent BeC12 and (2) 36.7 mol. percent KC1, 52.7 mol. percent LiCl, and 10.6 mol. percent BeC12; cell voltages of 0.30 to 0.80; and initial cathode current densities of 50 to 435 a./sq, ft. Current efficiencies ranging from 87 to 96 percent were obtained. Qualitative spectrographic analyses of the metal products indicated that impurities were reduced. This technique offers the possibility of producing a grade of beryllium purer than that now generally available, which may have better mechanical properties.

Jan 1, 1960

By T. L. Joseph

The purpose of this article is to describe briefly the operation of a 6-ton blast furnace on a charge of bauxite, limestone, iron ore, and cast-iron turnings and to point out the bearing which smelting such a charge has upon the production of alumina cement. One object of the experiment, conducted by the Bureau of Mines in cooperation with the Aluminum Co. of America, was to determine whether tae so-called Pedersen process3 can be applied to the blast furnace. This process consists of smelting a charge of bauxite, iron ore, and. limestone, and results in to products. One is a slag containing about 50 per cent of A1203 and is intended for use in manufacturing aluminum, and the other is iron low in sulphur. Complete details of the test are published in other reports4. Blast-furnace slag is now recognized as a satisfactory and economical raw material for making Portland cement, Wm. A. Forbes5 has recently reported that in 1926 an important steel interest used well over 1 million tons of slag in producing about 24 million long, tons of cement. This is equivalent to about ½ ton of slag for each ton of cement. Alumina cement can be made direct in the blast furnace. Its physical character would have to be changed by grinding, but no change in its chemical composition would be necessary.

Jan 1, 1928

By George D. Drechsler

The purpose of this review is to provide an analysis of the supply and demand for coal in Europe in 1955-56 and estimates of future growth in European requirements as a medium for appraisal of the effects and benefits to the economy of the United States. This review stems from observations and evaluations made in contacts with Government and industry representatives of the principal countries of Europe and is based on detailed data selected from the established flow of unclassified economic and statistical material originating in overseas areas for use and deposit in the Bureau of Mines, Foreign Solid Fuels Section. This material includes current reports and analyses prepared by the United States Foreign Service, official reports of individual countries, foreign industry and trade publications, and the committees of the several European organizations engaged in continuing review and study of problems relating to fuels and energy. The review is presented in four sections: 1. Discussion of the more important factors relating to the present and future fuels and energy position of Western Europe.

Jan 1, 1957

Use controlled blasting techniques to reduce blast-produced overbreak damage to underground mine ribs and back for both safer working conditions and improvements in productivity. The Problem Blasting is used in metal and non-metal underground mine slopes, drifts and crosscuts to fracture rock to be excavated and further processed. Standard blasting also produces fractures in the rock beyond the desired excavation area. This is sometimes evident by rough surfaces, undercutting and other signs of excessive damage. This damage contributes to rockfalls in the mines, a major cause of injuries and fatalities, and equipment damage. A variety of controlled blasting techniques has been developed for civil engineering projects where long-term stability is essential. For several reasons, these methods arc not widely used in mining. For example, these methods incur additional costs and time; there is little need to maintain stable openings over long periods of lime; and there is the perception (hat corrective remedial techniques, such as rock bolting, are more practical. Basically the benefits of these methods are not demonstrably clear for application in underground mines.

Jan 1, 1991

By D. G. Foot

The Bureau of Mines devised a direct flotation method for recovering potash from carnallite (KC1?MgC12?6H20) ore characterized by a high content of water-insoluble impurities. The method includes (1) a decomposition leach of the carnallite, (2) flocculation-depression of the insoluble slimes, (3) potash rougher, cleaner, and recleaner flotation, and (4) final product leaching. The technique eliminates the necessity for removing the water-insoluble slimes by mechanical or flotation de-sliming. Laboratory results demonstrated that the direct flotation procedure, when compared with conventional techniques, yielded equivalent or improved flotation results with equal or less reagent consumption. Locked-cycle testing of the direct flotation method recovered 87.8 pct of the potassium in the flotation feed in a final product containing 60.6 pct K20. A flowsheet incorporating the carnallite leaching-potash flotation procedure is presented.

Jan 1, 1982

By H. M. Smith

In studying the chemistry of lubricating-oil fractions from so-called ?paraffin-base? crudes, one of the first requisites is a method for the separation and removal of waxy material. A method utilizing solvents for this purpose is described in this report, together with preliminary experiments with solvents that led to its development. The solvents actually used are secondary butyl alcohol, acetone, and mixtures of these.. Isopropyl alcohol was also studied. Preliminary Experiments In previous work on "intermediate-base" crude oil, following the work of Wyant and Marsh acetone had been used for laboratory separations of oil and wax. Then acetone was tried for the separation of the waxes and oils of "paraffin-base" crude, the volume of acetone required (80 parts to 1 part of oil) was found to be too great for large-scale work. For this reason the effectiveness of other solvents was studied; the separation by acetone, however, was used as a standard.

Jan 1, 1927

By T. A. Lang

The objective was to develop a Program Plan of analytical studies and tests for determining (1) the optimum installation tension of a coal mine roof bolt, (2) the most valid bolt support theory or theories, and (3) the most valid roof failure theory or theories. On this basis a comprehensive literature search was made and significant material dealing with coal mine roof behavior, roof bolting and roof support was collected, reviewed, classified and analyzed. Emphasis was given to the influence of rock reinforcement on the control of deformation, stress field modification and mine roof stability. An assessment was made of the effect of various parameters including bolt tension, bolt pattern and time of installation, on the effectiveness of rock reinforcement systems, and equations developed for bolt tension as a function of these parameters, and rock properties. From these studies, a major program plan of tests and studies was developed for verifying and validating the most tenable theories of roof behavior and roof support and for determining optimum bolt installation tension.

Jan 1, 1979

By John R. Benham

The West Pioneer RARE II study area, No. 1-006 (fig. 1), has Figure 1.--NEAR HERE a high molybdenum resource potential. Two molybdenum-bearing areas are being explored by Utah International and by Cyprus-Moly Corp, Inc. using geophysical exploration and diamond core drilling. The study area also contains potential resources of gold and silver at six prospects: the Bear Paw (Ibex), Black Bear, Coeur d'Alene, Franklin No. 1, Martin, and Maynard. In addition, the Black Rear and the Martin contain possible copper, lead, and molybdenum resources. Most of the workings are caved.

Jan 1, 1981

By G. R. Hopkins

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Jan 1, 1927

By E. C. Perkins

This report describes a ferric chloride trap, based on formation of a low-melting sodium chloride-ferric chloride mixture of near-eutectic composition, and its use in chlorination of impure titaniferous materials. The trap is placed in the hot gas stream between the chlorination reactor and the condenser. Virtually all of the iron is removed by the trap. The condensed titanium tetrachloride is free of suspended solids and contains only a trace of iron. Four examples are given of the use of the ferric chloride trap in chlorination of impure titaniferous materials. INTRODUCTION In the Kroll process, ductile titanium metal is produced by reducing titanium tetrachloride with magnesium metal.4/ In commercial practice, titanium tetrachloride is produced by chlorinating titaniferous materials in the presence of carbon.2/ In 1957 most producers were using rutile, and virtually all plants were designed for its use. About four-fifths of the domestic consumption of rutile was imported from Australia. The Bureau of Mines, under provisions of contract DMP-116 with the General Services Administration, studied electrosmelting of domestic ilmenites and titaniferous magnetites to produce high-titanium slags with pig iron as a byproduct. Under the same contract, chlorination studies also were being made of these slags. Smelting was done at the Northwest Electrodevelopment Experiment Station, Albany, Oreg., and chlorination at the Electrometallurgical Experiment Station, Boulder City, Nev.

Jan 1, 1958

By William A. Beck

"The Old Cline mine, also known as the Old Cruse mine, was first worked for gold in1895. The property was opened by several shafts and trenches; and some stoping has been done, producing several cars of copper-gold ore in the early nineteen hundreds. Chalcopyrite is visible in selected samples; and, with the aid of a mineralite, several samples showing a considerable amount of scheelite were found on the old waste dumps.The mine is in Township 6, Cabarrus County, N. C., 5 miles north of the village of Mount Pleasant, 10 miles northeast of Concord, and about one-half mile south of Watts Crossroads. It is one-fourth mile east of the county road.When examined, the property was owned by H. F. Tompkinson, Concord, N. C., and was leased, with option to buy, by L. Nash. Titles of record were not investigated.As stated above, the Cline mine was first worked in 1895. The property was Purchased in 1902 by J. A. Clark and A. A. Smith of Atlanta, Ga., and worked for gold and copper. No record is available of the quantity of ore removed during these operations.A Bureau of Mines mining engineer3/ examined the mine as, a copper prospect on October 13, 1944.The Cline mine is in an area characterized by flat to rolling topography, dissected by many streams and rivers. It lies in the Piedmont Plateau and Varies in elevation from 700 feet to 800 feet. The surrounding country is partly wooded and partly cleared farm land.A quartz vein occurs in country rock of quartzite and greenstone.4./ The ore occurs in a series of quartz lenses, having a width of 1 to 3 feet and dipping about 750 NE, and striking N. 300 W. All these lenses have fairly sharp boundaries and in some cases are entirely separated from each other, while at other times they are connected by thin stringers of quartz. They can be traced for 1,000 to 1,200 feet by a series of shafts and test pits."

Apr 1, 1946

By A. B. Coates, J. E. Crawshaw

"The use of such methods and apparatus as the Dautriche method and the Mettegang recorder for the determination of the rate of burning of black blasting powder and other strictly burning explosives has been found to give such erratic results that no reliance can be placed on the data thus obtained. Consequently, investigators of those factors which may affect the burning rate, such as size of grain, absolute density, chemical composition, and means of ignition have had to rely mainly on observations made during practical use for determination of the part played by each. Such tests are very difficult of interpretation.The purpose of this paper is to describe a method used by the explosives division of the Bureau of Mines for the investigation of such explosives and to present the results of an investigation using that method.The investigation was concerned with the effect of grain size, initial pressure, and means of ignition on the rate of burning or rate of pressure development of black blasting powder as compared with pellet powder.The Bichel pressure gauge was used for these tests, with the slight modification to the apparatus and method described in U. S. Bureau of Mines Bulletin 15.4 These modifications consisted of reducing the speed of the revolving drum on which the time-pressure record is taken, measuring the speed of the drum by a belt-driven tachometer, and introducing an induction coil in series with the electric squib or electric detonator to mark on the time pressure record the instant at which the squib or detonator was fired."

May 1, 1929