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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 Jeffery M. Listak, Ernest A. Curth

"It took only 9 years from the first appearance of roof shields on the U.S. longwall mining scene to the present predominance of shield faces. An apparent consequence is the welcome downward trend in accidents related to failures in longwall ground control. The report addresses load prediction, the effects of shield geometry on support loads, factors contributing to ground control, and related techniques. The Bureau of Mines took an active part in the evolution of longwall mining, including developing one of the first shield faces in 1975, the first lemniscatetype shields in 1976, the Mine Roof Simulator completed in 1980, the first shields in steeply pitching coalbeds in 1981, and the first multilift working of a thick coalbed in 1982. The information offered in this state-of-the-art report will assist in establishing criteria for roof support selection. INTRODUCTIONIn terms of roof support technology, the introduction of shields in the seventies and eighties was a major step forward. Table 1 indicates the predominance of shield faces on the U.S. longwall mining scene and its apparent consequence, a welcome downward trend of ground-control related accidents.The rapid progress of longwall technology began in 1975 and is highlighted by a development leading from the caliper shield to the modern lemniscate type. Shields have been gaining preference over chocks since their advent to longwall mining in 1975. Safety and productivity factors favoring shields over chocks are--1. A sheltered working space requiring minimum cleanup work.2. Structural stability that allows advancing without delay even with brushing roof contact and, by controlling all lateral loads, removing the requirement for cumbersome leg restraint and restoration devices.3. Wide hydraulic range of mining height.The development of roof shields in the Federal Republic of Germany preceded and paralleled their rapid adoption by U.S. miners. In 1983, 87 pct of the total production in Germany came from shield faces (1).2 In Great Britain, the National Coal Board introduced the first shield support system in 1977 to initiate Advanced Mining Technology (ATM) and Heavy Duty Mechanization (HDM) programs; as of mid-1982, 44 shield faces were operating, or 7.5 pct of a total of 581 faces CJ_)."

Jan 1, 1985

By A. D. Hahn

This report describes reconnaissance by the Federal Bureau of Mines of titanium-bearing sandstone in Kemper County, Miss. The purpose was to determine the ilmenite, rutile, and associated heavy-mineral content of black-sand-bearing Eocene deltaic formations" The investigation was part of a survey of titanium resources of the United States. Ilmenite (FeTi03), an iron-titanium oxide, is the major titanium-bearing mineral consumed in the titanium pigment industry. Rutile (Ti02), titanium oxide, is used mainly in producing welding-rod coatings and titanium metal. The fieldwork was conducted during the first half of November 1959. Seven holes, totaling 304 feet of bore, from which 64 samples of cuttings were taken, were drilled in the north-central part of the county; and two holes, totaling 172 feet of bore, from which 34 samples of cuttings were taken, were drilled in the southeastern part.

Jan 1, 1961

By Dougherty. E. Y., S. W. Zoldok, John W. Cole

"INTRODUCTION During its wartime program of exploration for minerals essential to the national economy, the Bureau of Mines was instructed to investigate sources of raw materials used in the manufacture of iron and steel. As a part of this investigation, some work was done on the iron deposits on the Neutral and Aztec claims on Buckhorn Mountain Canogan County, Washington, which was designed chiefly to indicate the nature and behavior of the ore deposits below the surface exposures. Diamond drilling was started in June and completed in July 1945. Preliminary laboratory tests on iron, ore from Buckhorn Mountain were completed during the fall and winter of 1945. This report presents the data obtained from the investigation.ACKNOWLEDGMENTSIn its program of exploration of mineral deposits, the Bureau of Mines has as its primary objective the more effective utilization of our mineral resources to the end that they make the greatest possible contribution to national security and economy. It is the policy of the Bureau to publish the facts developed by each exploratory project as soon as practicable after its conclusion. The Mining Branch, Lowell B. Moon, chief, conducts preliminary examinations, performs the actual exploratory work, and prepares the final re¬port. The Metallurgical Branch, R. G. Knickerbocker, chief, analyzes samples and performs beneficiation tests."

Apr 1, 1947

By Byron E. Blair

This report describes procedures for using a high-speed camera to study blasting phenomena. Both quantitative and qualitative information can be obtained, provided that proper interpretations of the projected two-dimensional images are made. Geometrical relationships between object and image displacements are given in terms of horizontal and vertical angles of the camera optic axis with respect to the quarry face. Correction factors are given for obtaining true object displacements from image displacements in the camera film plane. The time of initial rock movement also is considered, and the control-ling factors of camera speed, scale factor, minimum increment of projection measurement, etc., are evaluated in terms of minimum time intervals. The high-speed camera and associated equipment are described, and field measurements and laboratory data analysis techniques are outlined. An analysis of a typical high-speed motion picture is made, and the application of the necessary correction factors is illustrated.

Jan 1, 1960

By A. W. Deurbrouck

This Bureau of Mines report describes the preparation characteristics of the significant coalbeds from which samples could be obtained in Upshur County, W. Va. One of the 14 samples collected was of metallurgical quality as received, 6 could be sufficiently upgraded to provide acceptable products, and 7 could not be upgraded to metallurgical quality because of their high sulfur contents.

Jan 1, 1967

By NIOSH NIOSH

This work explores application of a double alkaline leach method to extraction of alumina from Oregon ferruginous bauxitic materials. The process recovers a greater proportion of alumina from high-silica ores than is possible by a conventional single-leach method. This recovery is accomplished by calcining the ore, removing reactive silica in a preliminary dilute caustic soda leach, and then applying a second leach to dissolve alumina. Ores containing up to 15 percent Si~) 35 percent AI;:) Os, and 30 percent Os were examined. Under conditions of treatment established by experimentation, more than BO-percent alumina extraction was demonstrated. When and if conditions demand the use of low-grade materials, the double-leach process is capable of providing millions of tons of alumina from Oregon ferruginous bauxite.

Jan 1, 1963

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 B. W. Madsen

Research by the Bureau of Mines has shown that treatment of open pit waste by crushing and sizing followed by flotation of the fines and leaching the coarse fraction results in greater metal recoveries than obtained by leaching only. Tests with a chalcocite-bearing quartz monzonite mine waste sample that had been crushed to minus 6 inches and screened on 1/2 inch yielded copper and silver recoveries of 71 and 22 percent, respectively, by the combined flotation-leaching process, compared with 48 percent of the copper and no silver recovered leaching the run-of-mine material. Copper was more readily leached from the coarse material with the minus 1/2-inch fines removed than from material with the fines included. The improved leaching was attributed to improved permeability and the associated improved circulation of air to the interior of the ore column. Cost estimates showed that the proposed intensive treatment of mine waste will require a greater capital investment and higher annual operating costs than conventional milling and dump leaching process. However, the income from the additional metal production offsets the increase in capital investment and operating costs, resulting in additional profit.

Jan 1, 1975

By B. W. Gandrud, G. D. Coe

"INTRODUCTION The Southern Experiment Station of the U.S. Bureau of Mines, cooperating with the University of Alabama and Alabama coal producers, has made a series of investigations of the washability of coal from commercially important bens of Alabama. The results of 13 investigations pertaining to the Mary Lee, Clark, Black Creek, Jefferson, Pratt, Corona, Carter Brookwood, Blue Creek, Thompson, and Woodstock beds have been published. 4/ This report, the fourteenth of the series, deals with run-of-mine coal from the Henry Ellen bed at the Acmar No. 5 mine of the Alabama Fuel & Iron Co.The Acmar mine is 1/2 mile west of Acmar, Saint Clair County, in the northern part of the Cahaba field. Present production at the mine is about 800 tons per day, all of which, accept the lump coal, is treated in jigs. The washability data were obtained by means of screen-sizing and float-and-sink tests. There are included, also, tests showing the extent of liberation of impurities by recrushing the coarser sizes of coal from the top bench and tests showing the flakiness in selected sizes.SAMPLING AT THE MINEThe Henry Ellen bed at Acmar consists of two benches separated by a shale parting. At the point of sampling the top bench was 6 feet 3 inches thick and contained a 1-inch and a 1 1/2-inch band of bone. The bottom bench was 5 feet thick and was separated from the top bench by 20 inches of shale. In taking the samples for the washability study the working face was squared up, and a representative 2-ton section was out from each bench. The shale parting was discarded, according to usual mining practice."

Nov 1, 1936

By James W. Miller

An investigation was begun by the Bureau of Mines in 1948 to determine the preparation characteristics of American coals. Results of the investigation were planned to be reported on a county basis and from the data developed, to determine: (a) Which coals either as mined or after beneficiation by conventional preparation are chemically suitable under present standards for producing metallurgical coke; (b) Which coals require special and more intensive treatment in preparation than is now practiced; and (c) Which coals cannot be considered potential sources of metallurgical coke, regardless of preparation. This report is one in this county series that describes the preparation characteristics of the coals of Perry County, Ky.

Jan 1, 1956

By J. H. Jacobs

The first authorization, in November 1940, was for a plant of only several hundred pounds capacity at Boulder City, Nev. Improvements in the process and subsequent additions to some sections have enabled the plant to produce more than 2,000 pounds of manganese per day for substantial periods. By the time pilot-plant operations were suspended in June 1945, over 1,500,000 pounds of metal had been produced. The future of electrolytic manganese production obviously depends not only on satisfactory development of methods but on availability of raw material and demonstration of valuable uses. Investigations of manganese-ore deposits in this country, made since 1938 by the Bureau of Mines, have revealed large amounts of ore suitable for making electrolytic manganese. At first the pilot plant was operated on ore from the Three Kids mine near Las Vegas, Nev. After practical features of the process had been worked out, other ores from throughout the United States were tested in the pilot plant. The purpose of this paper is to compare the results obtained on the following ores: Three Kids; Ladd mine, Tracy, Calif.; Chamberlain, S. Dak., nodules; and ore from Metals Reserve stockpiles at Deming, N. Mex.; Cushman, Ark.; and Philipsburg, Mont.

Dec 1, 1947

By R. V. Lundquist, H. Leitch

The solubility characteristics of mono calcium aluminate (CaO A₁₂ 0 ) in water and in NaOH , Na₂ CO₂ , and NaOH - Na₂ CO₂ solutions were measured by determining the changes in Al2O3 concentrations in solution over a period of time at a specified temperature . The monocalcium aluminate was synthesized by sintering its starting components for 72 hours at 1,375 ° C. Distilled water and aqueous solutions of technical grades of NaOH and Na₂ CO₂ were used as solvents . The extraction of alumina from the monocalcium aluminate was dependent on the composition of the solvent and partially dependent on temperature for leaching . About 98 percent extraction of alumina from the aluminate occurred in Na₂ CO3 solutions containing 10 to 12 percent NaOH . Other solution compositions produce lesser extractions .

Jan 1, 1963

By J. H. Field

Results of studies by the Federal Bureau of Mines on a pilot-plant scale for removing hydrogen sulfide and carbonyl sulfide from gas mixtures by the hot carbonate system are given in this publication. Gases containing up to 10 pet. hydrogen sulfide and 48 grains carbonyl sulfide per 100 cu.ft. were treated. In most tests carbon dioxide also was present and was removed simultaneously with the sulfur compounds. Because the rate of absorption of hydrogen sulfide is much more rapid than that of carbon dioxide over a wide temperature range, selective removal of hydrogen sulfide occurred in the bottom section of the absorber near the point of gas entry. Hydrogen sulfide was removed to pipeline specifications with carbonate solutions by using split-stream flows in the absorber and regenerator.

Jan 1, 1960

By Louis C. Brichta

The Capital Mine is one of, the more important zinc mines in Lawrence County, Mo. Owing to the urgent need for additional zinc during the war and the available facilities for the treatment of zinc-lead ores at the property, the Bureau of Mines examined the mine during July and August 1942 and selected it for further investigation by churn drilling, which was accomplished in the fall of 1943 and spring of 1944. At the conclusion of the drilling on the Capital holdings, the Greenland property, immediately south, was investigated by drilling two additional holes. Results of the investigation are presented in this report.

Jan 1, 1948

By A. L. Peyton

The Brewer mine, near Jefferson, Chesterfield County, S. C., was originally operated as a gold mine. As late as 1890 this mine was reported to have been one of the large gold producers in the southeast. Occurrence of topaz on the Brewer property was not reported until 1935, when it was discovered, by Parks3/ and Parks of the Federal Geological Survey while they were investigating gold deposits in the Piedmont province.

Jan 1, 1953

By G. A. Appell

"INTRODUCTION During the summer of 1945, the Bureau of Mines conducted an investigation and program of churn drilling near the village of Tennyson in Grant County, Wis. The work was undertaken as part of a general investigation of the zinc-producing area of southwestern Wisconsin at a time when all effort was being made to increase the production of metals important to the war program.The area for special investigation was selected on the basis of favorable structural disclosures, evidence of widespread zinc mineralization, absence of any great amount of exploration to depth beneath the productive shallow workings, and the favorable results of several churn-drill holes in the village of Tennyson.During the Bureau's investigation, 30 churn-drill holes aggregating5,888 feet were completed.ACKNOWLEDGMENTSIn its program of investigation of mineral deposits, the Bureau of Mines has as its primary objective the more effective utilization of our mineral resources to-the end that they make the greatest possible contribution to national security and economy. It is the policy of the Bureau to publish the facts developed by each project as soon as practicable after its conclusion. The Mining Branch, Lowell B. Moon, chief, conducts preliminary examinations, performs the actual. Investigative work, and prepares the final report.The work described herein was accomplished under the direct supervision of Francis C. Lincoln and the author, mining engineers of the Bureau of Mines. Final data on the investigation were prepared under the direction of Edward F. Fitzhugh, Jr., chief Minneapolis Division, Mining Branch."

Jun 1, 1947

By R. Hogg, T. F. Dumm

"A procedure for evaluating the size/specific gravity distribution of ultrafine coal and the distributions of sulfur and ash with respect to particle size and specific gravity is described. The procedure is essentially an extension of the conventional coal washability technique in which special precautions are taken to ensure particle dispersion in the heavy organic liquids, centrifuges are used to obtain adequate separation rates, and micromesh sieves are used for size separation at fine sizes. An example of the application of this technique to the evaluation of the extent of liberation of sulfur and ash in a coal sample ground to 90Z passing 200 mesh (74 um) is described.INTRODUCTIONIn order to determine the potential for deep cleaning of coal by fine grinding to liberate sulfur and ash-forming minerals, it is necessary to obtain data on the distributions of these species by size and specific gravity. In conventional coal processing operations, this information is obtained by means of a standard ""washability"" analysis. Attempts to extend this procedure to ultrafine coal, however, have generally been unsatisfactory and have often led to unreliable and inconsistent results [11. The present authors have described a modified washability procedure in which cumulative specific gravity fractionation is combined with sub-sieve size analysis (by laser diffraction/light scattering) to determine the particle size/specific gravity distribution of ultrafine coal [2]. Unfortunately, because this technique does not involve separation of the individual fractions, only limited information can be obtained on the specific distributions of sulfur and ash.The objective of the work described in this paper was to develop and evaluate a procedure for size and specific gravity fractionation of ultrafine coal and to use conventional analyses for sulfur and ash to determine their relative distribution in the coal. The procedure is essentially a simple extension of the standard washability analysis [3] but incorporating special precautions for treating ultrafine particles.EXPERIMENTAL Material The material used in the development and evaluation of the ultrafine coal fractionation procedure was a medium volatile bituminous coal from the Lower Kittanning seam. A sample of the coal (nominally - 1/4 inch), obtained from the Penn State Coal Data Base, was ground to 90% passing 200 mesh by the following two-stage grinding procedure: About 2 kg of the as-received coal were ground to about 30Z passing 200 mesh in a Model 4-E Quakertown mill (""coffee grinder""). About 1 kg of this product was then ground to about 90Z passing 200 mesh in a Holmes Model 300 Pulverizer."

Jan 1, 1989

By Thomas A. Jones

An impure variety of barite, which lends itself well to the manufacture of heavy drilling mud for oil wells, is widely distributed throughout the Ouachita Mountains in Arkansas. The ore mined in the area and used for drilling muds usually contains an average of 67 percent barium sulfate, although ores as low as 50 percent BaSO4 are occasionally used. Due to the increased demand for barite for drilling caused by the intense search for hew oil occurrences during the years 1945 and 1946, the Federal Bureau of Mines began an investigation of barite deposits in the Ouachita? Mountains in October 1946. In all, 10 barite deposits were examined, trenched, sampled, and studied during the investigation, which was terminated in May 1947.

Jan 1, 1948

By Jr. East

The Bureau of Mines conducted an investigation of the Nightingale tungsten deposit about 38 miles north of Fernley, Nev., from September 1939 to March 1940, to determine possible resources of tungsten ore. The property was owned by the Gold, Silver & Tungsten, Inc., which maintained its offices in Boulder, Colo. Ore was discovered in 1917, and some ore was mined in 1918 and treated in a mill at Toulon, a station on the Southern Pacific Railroad, 40 miles east. Same shipments were made since 1918, but no production figures are available. The ore is mined from nearly vertical tactite bodies at the limestone-granite contact. The Bureau of Mines excavated 944 linear feet of trenches, drifted 52 linear feet, sunk a shaft 20 feet in depth, sampled the underground workings by cutting 743 linear feet of channels, sampled the surface trenches by cutting 415 linear feet of channels, and drilled 9 diamond-drill holes, totaling 3,000 feet. The ensuing sections note the location and physical features of the district and specify the property and ownership. The history of the mine is briefed, and the geology and mine workings are described. The work done by the Bureau of Mines is summarized and supplemented in detail by assay maps, logs of diamond-drill holes in appendix A, and a table of sample analyses in appendix B.

Jan 1, 1950