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By M. H. Kersten, G. A. Brady, Jerry W. Ramsey

Anthracite samples were oxidized with nitric acid to prepare products representing intermediate stages of oxidation . Similar oxidizing conditions affected different anthracites to varying degrees as characterized by peptization behavior with 0.1 N NaOH . Techniques used in attempts to separate and characterize the products included esterification , absorption spectrophotometry , sublimation , chromatography , electrophoresis , metal salt formation , and solvent extraction . Mellitic acid , either free or in the form of metallic salts , was identified in the acid- soluble products from 10 tests in which the anthracite was treated with nitric acid for periods varying from 24 to 1,000 hours . pentacarboxylic acid was also found in some products . Other benzene carboxylic acids were not present in amounts detectable by the methods used in this study . The acid- insoluble residue from nitric acid treatment varied significantly in solubility behavior toward different classes of solvents . The most effective ones tried included polar oxygenated solvents and pyridine . Infrared spectra of the extracted material indicated that similar compounds were extracted by the different solvents . Aliphatic amines and aniline peptized the residue and o- toluidine reacted with it . Organic material separated from the residue by peptization with dimethylformamide contained 1 percent ash , consisting of more than 50 percent zirconium .

Jan 1, 1964

By J. E. Pahlman

Spontaneous oxidation and combustion of sulfides and resultant fires are serious problems in underground mines. The Bureau of Mines has con-ducted fundamental thermal gravimetric analysis (TGA) research to deter-mine the mechanisms and factors governing the rate of low-temperature pyrite oxidation, and to identify possible inhibitors to spontaneous oxidation and combustion. The mechanism of low-temperature pyrite oxidation was found to be topochemical, meaning that the oxidation process is controlled by the chemical reaction at the interface between pyrite (FeS2) and iron sulfate (FeS04)' An activation energy of 8.9 kcal/mol FeS2 was obtained for oxidation of minus 500-mesh pyrite in an atmosphere of 60 vol pct water vapor and 40 vol pct . Water-vapor content of the atmosphere was found to be the critical factor in the rate of spontaneous oxidation of pyrite, with a water-vapor content greater than 20 vol pct needed for accelerated oxidation. An atmosphere of pure oxygen resulted in negligible oxidation. The rate of pyrite oxidation is also greatly affected by the particle size of pyrite. Pyrite-oxidation rate increased drastically for particles less than 40 ~m. Room-temperature pyrophoric behavior was observed for freshly ground unoxidized pyrite (55 pct minus 5 ~m) upon exposure to air. Addition of water-adsorbing materials such as activated alumina (Alz03) decreased the rate of pyrite oxidation.

Jan 1, 1986

By F. E. Joyce, Charles Prasky

This report describes the response to high- temperature sulfatization of a variety of manganese minerals and companion compounds which may occur either as a principal component or as a gangue material in low- grade manganese deposits . Fourteen manganese samples representing oxide , carbonate , and silicate minerals as well as seven compounds which might occur as gangue with manganese minerals were tested batchwise in a bench- scale apparatus under conditions which would be favorable for the sulfatization of manganese . The manganese minerals substantiated thermodynamic predictions and responded to sulfatization but to varying degrees . The gangue materials , MgO , MgCO,, CaO , and CaCO3 , were sulfatized readily in contrast to the iron oxides and the aluminacontaining material which were not .

Jan 1, 1964

By Manuel Gomez

This report presents low-temperature tar data from studies by the Bureau of Mines of tars produced in an externally heated (entrained state) pilot-plant-scale retort. Analytical data covering 20 low-temperature tars, derived from the. carbonization of various ranks of foreign and domestic coals, are tabulated. The character of the tar is discussed in relationship to carbonizing conditions and the rank of coal. It is seen that in carbonization techniques that employ entrainment or fluidization of the coal particle, carbonization conditions are secondary to coal rank with respect to tar-oil yields and composition. The influence of distillation conditions on recoverable yields of tar products is presented. The probable yield of commercially important chemical products, based on a ton of pure (moisture- and ash-free) coal, are predicted. INTRODUCTION Low-temperature tars produced by entrainment or fluidized carbonization techniques that employ internally heated reactors represent the most nearly primary tart produced by industrial processes. In brief, such a process involves the application of a heat gradient to the coal particle "boiling" or suspended in a turbulent state in the reactor chamber. Conditions are observed so that the coal particle remains suspended within the reaction zone by a gas stream for a time interval commensurate with maximum tar-oil yield. The heat necessary for the carbonization reaction may be obtained entirely from the hot (preheated) gas stream, or it may be derived partly from the combustion of the volatile products and char by the transport gases, usually air. The volatile material moves out of the carbonizing zone at a rate that approaches the velocity of the transport gas. Carbonizing conditions are ideal when a minimum particle residence time is obtained within the reactor at a given temperature and a maximum yield of condensable volatile matter is released. In industrial practice this objective is a compromise.

Jan 1, 1957

By Kenneth J. Miller

The Federal Bureau of Mines coal-pyrite flotation process has been modi¬fied to produce a concentrated final clean coal slurry underflow that could be dewatered more effectively by filtration or centrifugation. This change was accomplished by redesigning the Bureau's two-stage flotation pilot plant facility and running the second-stage flotation step with undiluted or only partially diluted first stage coal froth concentrate. Results of the pilot plant flotation tests showed that substantial sulfur reduction could be achieved by flotation with undiluted pulp but some dilution is recommended for maximum selectivity. For example, coal-pyrite flotation in slurry of 25 percent solids yielded clean coal products analyzing as low as 0.7 percent pyritic sulfur and froth reject products containing slightly over 3.0 percent pyritic sulfur. In comparison, coal-pyrite flotation with pulp diluted to about 12.5 percent solids yielded clean coal containing as low as 0.4 percent pyritic sulfur and froth reject of 5.6 to 6.7 percent pyritic sulfur. Despite the need for some dilution, it was concluded that excellent coal-¬pyrite flotation selectivity could be achieved without diluting to 6 or 7 per¬cent solids as done in the earlier work. Thus the economics of coal-pyrite flotation would be improved by easing clean coal dewatering problems and by reducing second-stage flotation cell volume requirements.

Jan 1, 1977

By A. W. Fahrenwald

"About two years ago the Bureau of Mines, Department of the Interior, and the University of Idaho undertook an investigation of classification in its relation to table concentration of Idaho ores. The cooperation of the management of the Bunker Hill & Sullivan Co. in placing at our disposal their West Mill and facilities as desired, offered an unusual opportunity for studying the field of hindered classification in its practical and economic relation to table concentration.It has been shorn theoretically, and demonstrated experimentally, that ore products are more easily and economically concentrated on tables if the natural feed, consisting of various minerals and of all sizes of particles of each mineral, be classified or grouped into a series of products in which the mineral particles of greatest density are small in diameter relative to the diameter of the mineral particles of lesser density. Products in which the maximum difference in diameter of light and heavy minerals occurs are to be obtained only by true hindered settling classification. To our knowledge there has never been a really good hindered settling classifier used in practice and the present tendency seems to be to by-pass any attempt at such classification.After a careful study of the nature of hindered classification and of the requirements for hindered settling in practice, a classifier has been developed that takes fullest practical advantage of the widely known, but generally only meagerly understood, condition of hindered settling so well analyzed a number of years ago by Dr. Richards.The present paper presents briefly some of the more important practical results accruing through the investigation."

Jun 1, 1924

By G. W. Birge

This report describes the carbonizing properties of the principal coal beds of McDowell County, W. Va. Coals from 14 coal beds were selected for study: Upper Cedar Grove, Middle Cedar Grove, Lower Cedar Grove, Eagle, Douglas, Iaeger, Sewell, Welch, Beckley, Fire Creek and Pocahontas Nos. 3, 4, 5, and 9. Selection was based upon estimated minable reserves. McDowell County coals rank either as high-volatile A, medium-volatile, or low-volatile bituminous coal, and this variation in rank is reflected in the wide diversity of the carbonization properties of the coals. All coals tested were either satisfactory as mined or could be upgraded to meet present chemical standards for metallurgical coke; the coals produced strong coke, as determined by ASTM shatter and tumbler tests.

Jan 1, 1958

By Bernard J. Steblay

The U.S. Bureau of Mines has attempted to use ultrasonic signal travel-time measurements to measure loaded roof bolt strains. The strain measurements are then related to roof bolt loads through equations or empirical calibrations. Such techniques offer the potential of accurate, rapid bolt load measurement that does not disturb the anchotage. This report presents 6e research findings for a specific type of ultrasonic measurement instrument using a pulsed-phase-Iock-Ioop technique. This technique measures signal travel time indirectly by measuring frequency changes. A complete development of the applicable theory and detailed derivations of key equations is presented along with empirical laboratory and field results. The differences between anticipated and measured behaviors are analyzed and discussed. The report identifies problems encountered in applying pulsed-phase-Iock-Ioop technology to roof bolt load measurement and provides potential solutions to many of them. A key assumption of pulsed-phase-lock-loop theory is that driving and reflected signal frequencies will always be equal. Findings showed that not only were actual frequencies not equal but they were not stable or simply related. Reflection wave shape also was not stable. The ramification of these findings and ways to minimize their adverse effects are presented.

Jan 1, 1990

By D. S. Burgess

An investigation of the hazard of spillage of liquefied natural gas (LNG) onto water is described. About 2,000 gallons of LNG were consumed in various tests. The initial vaporization rate of LNG following spillage was found to be 0.037 lb/ft2 sec; when the spill was confined, this vaporization rate was moderated after about 20 seconds by the growth of an ice layer on the water surface; when the spill was unconfined, a coherent ice floe was not observed and the vaporization rate was essentially time independent. The maximum diameter (in feet) of the spreading LNG pool was found to be given by 6.25 Wo 1/3, where Wo is the weight of LNG in pounds, Downwind of a natural gas source, time-averaged methane concentrations were given in good approximation by standard air pollution equations. However, peak concentrations were as much as twentyfold higher than average, adding an additional factor to the assessment of hazard. The effect of layering by the cold vaporized natural gas was similar to the effect of a temperature inversion on normal gases in the atmosphere. Small-scale explosions were observed on pouring LNG onto a water surface; no single explanation seems pertinent to all of the incidents observed.

Jan 1, 1970

By Joseph A. Sutton, John D. Corrick

The chemistry involved in the microbial dissolution of iron and copper from such sulfide minerals as pyrite, chalcopyrite, chalcocite, cove11ite, and bornite is described. The chemical criteria used to evaluate the activity of microorganisms on these minerals were changes in pH, ferric iron produced, and oxygen consumption. In a series of experiments in which a ferrous sulfate nutrient solution was percolated over small portions of the above-mentioned copper sulfide minerals for 56 days, the iron-oxidizing bacteria Ferrobaci11us ferrooxidans and Thiobaci11us ferrooxidans were capable of bringing about the dissolution of 23.7 percent of the copper from chalcocite, 56.3 percent of the copper from cove11ite, and 29.8 percent of the copper from bornite by the microbial production of ferric sulfate which reacted with these minerals. Laboratory tests have demonstrated that pure strains of the iron-oxidizing bacteria act as catalysts to the ferrous iron being oxidized by the Oxygen of a system containing pyrite and chalcopyrite. In a series of experiments during which nutrient solution was percolated over pyrite for 70 days, the ferric iron produced by the iron-oxidizing bacteria was 112 to 120 times greater than that produced atmospherically.

Jan 1, 1964

By E. C. Baker

The capital investment and operating costs of two methane-control systems used during longwall mining operations are compared in this Bureau of Mines report. Costs are given for a surface gob hole drainage system and an underground cross-measure borehole drainage system to control methane gas in gobs in four coal mining areas--central Pennsylvania, northern West Virginia, southern Virginia, and northern Alabama. Present-worth analysis is used to determine the more cost-effective alternative in each location. The alternatives have equal lives and provide the same service based on a minimum rate of return of 15 pet. In central Pennsylvania and northern West Virginia, the gob hole system is more cost effective than the cross-measure system, by 10 and 18 pet, respectively. In southern Virginia and northern Alabama, the cross-measure system is more cost effective, by 29 and 38 pet., respecitively. Costs for other locations must be developed on a case-by-case basis.

Jan 1, 1988

By Paul G. Swanson

This manual of practice is to be used in combination with the final reports for the study of spoil stability in the Eastern Coal Province. The manual applies the predictive matrices developed in the parent study for use in evaluating the stability of typical mine spoil slopes. The values of internal friction and pore pressure coefficient are derived for many varied slope conditions. The results can be used in conventional stability analysis equations to assist the mine operator or regulatory personnel in evaluating spoil stability from very limited information.

Jan 1, 1983

By J. A. Eisele

The Bureau of Mines is investigating the recovery of alumina from domestic nonbauxitic resources, including anorthosite. The United States has large reserves of anorthosite, but its aluminum content is less than 50 pct soluble in acid, unless a source of fluoride is added to the acid. A flowsheet that includes leaching with HCl and fluoride followed by crystallization of AlC13.6H20 from the pregnant liquor by HCl gas injection was designed. Approximately 90 pct of the aluminum values were recovered from the anorthosite when a ratio of 0.14 mole of fluorine per mole of aluminum was used. Sodium chloride is cocrystallized with the A1C13.6H20 but is removed by water washing of the Al203 product. A material balance is given based on results of laboratory studies of the unit operations.

Jan 1, 1983

By Thomas Fraser

About 24 per cent of our total production of bituminous coal is used in industrial power plants. As regards fuel conservation, therefore, the recovery of unburned fuel from furnace refuse presents interesting possibilities. Considerable attention has been given to this problem in the past, but because of the comparatively low initial cost of power plant fuel in the pre-war period little progress, has been made in this direction in the United States. Because of the higher price of coal in Europe more attention has there been given to the problem. In Germany a process has been developed for separating unburned coal in refuse by using an electromagnetic separator In the United States the use of mechanical stokers enabled low-priced screenings of high ash content to be used, so that even with relatively high percentages of combustible material remaining in the refuse, the loss in money is not excessive. If the price of screenings returns to the pre-war level around $1.00 per ton the process proposed here will probably not be especially interesting, except where the freight charges are very high. However, if the price of delivered coal continues high, such a process should result in considerable saving. The cost of continuous operation of such a refuse treating plant should not exceed 75 cents per ton of fuel recovered.

Jan 1, 1921

By C. E. Augustine, B. A. Landry, P. Nicholls

"Wien bituminous coal is burned in a hand-fired up-draft boiler used for heating purposes it has a decided tendency to produce smoke. A design of furnace and a method of firing and attendance that are satisfactory for fuels low in volatile matter, as anthracite or coke, are not necessarily Satisfactory for bituminous coals. It is therefore becoming common practice to use a special design of furnace for bituminous coals, in order to facilitate the combustion of the volatile matter and soot. This is done by (1) providing a larger combustion space to give more time for the combustion, (2) construction that will produce a better mixing of the gases and secondary air supplied over the fuel bed, or (3) keeping the gases at a higher temperature by preheating the secondary air, as may be done by surrounding them with refractory surfaces, or causing them to pass through a fuel bed of hot coke. A furnace may be built to use any or all of these methods of smoke prevention.In Bureau of Mines Technical Paper 303, Blizard5 and others give tests on a large heating boiler when burning coke, anthracite, and bituminous coal. Certair alternative furnace arrangements were used, but there was no material change in the furnace design for the various fuels. Since that time the manufacturer has made modifications in design to adapt it for use of bituminous coal, and additional tests have been made to determine how this change affected the production of smoke and the efficiency of the boiler."

Jun 1, 1929

By Alfred R. Powell

In another paper the writer has described an investigation in which the forms of sulphur in coke were determined and described. Coke was found to contain four characteristic forms of sulphur- namely, ferrous sulphide, sulphates, ad- sorbed free sulphur, and sulphur held in solid solution in the carbon. While the coke is still in the oven, only two forms of sulphur are present namely, the ferrous sulphide and the sulphur in solid solution in the carbon. During the quenching, however, the sulphur of the coke is subjected to considerable oxidation, a portion of the ferrous sulphide being oxidized to free sulphur and sulphates, while the solid solution form remains unchanged. The coke, however, loses no sulphur during this process, since the free sulphur which is formed ie retained by the coke in an adsorbed form. Since this oxidation of the ferrous sulphide took place so easily, an inves- tigation was undertaken to determine whether this property could not be taken ad- vantage of in some industrial process for the desulphurization of coke. Although it is true that such a roasting process would not touch the solid-solution form of sul- phur, still the removal of the ferrous sulphide sulphur would undoubtedly benefit the coke from the standpoint of the metallurgist. This improvement in the coke would result not only from the decrease in total sulphur, but also from the large decrease in the ferrous sulphide, which is responsible for the contamination of the iron in the upper part of the blast-furnace. The de sulphurization of coke by roasting in air it a new idea, but dates back to the earliest days of coke manufacture. In 1871, Philipparts published the results of some work done by him on the de sulphurization of coke by air, as well as a review of the results of earlier investigators. In the se earlier experiments, nothing was known of the forms in which the sulphur existed in the coke, while the temperature measurements were only approximate, so that altogether the results were not very conclusive nor complete. The de sulphurisation figures given by the se early investigators generally showed a low efficiency for the process, but some extraordinary results were claimed by certain inventors. In the light of our new knowledge concerning the coke sulphur, it seemed to be important enough to warrant investigation.

Apr 1, 1923

By Clarence O. Babcock

In this report, the Bureau of Mines presents a method for reducing the complexity of designing room-and-pillar mining systems by treating them as anisotropic soft inclusions in the surrounding ore or host rock. Theoretical models were derived for the calculation of the effective Young's moduli for these systems. The predicted behavior of the plate-type elements used in these models agreed well with test results from 21 plates each with 49 holes spaced on a 7 X 7 Cartesian grid. The plates behaved as anisotropic solids, the effective Young's moduli of which could be predicted from the scaled hole size and spacing. Actual hole shape was insignificant. The effective Young's moduli for simple mining systems are calculated in sample problems. This approach should provide information about field stress in the mining region and the stress distribution in the surrounding ore or host rock when the actual mining configuration is replaced by an anisotropic inclusion in a finite element analysis. The field stress within the inclusion can then be applied to the actual opening shape to determine the stress distribution within the mining region.

Jan 1, 1970

By H. B. Humphrey, F. E. Cash

The Birmingham coal-mining district of Alabama has many local physical conditions that contribute largely to the proble of preventing coalmine fatalities . Coal : nes of Alabama have been under the supervision of the State mine inspector since 1892 , and reports have been made with increasing completeness since that time . The U. S. Bureau of Mines has maintained a station of the safety division in the district since 1912 to cooperate with operators and the State in the advancement of safety in mining . A description of conditions in regard to fatal accidents as they have been and as they now are in Alabama , compared with the entire United States , will indicate the progress that has been made and that should still be made in reducing fatal mine accidents .

Sep 1, 1930

By Roy J. Greenfield

The overall purpose of this research was to improve the understanding of how the post disaster seismic location system works, what determines the signal size, what is the character of the seismic noise, how well the system can detect blows from a trapped miner, and how well the source of the blows can be located. Based on an improved understanding of the system, improvements were suggested in the seismic subarray configuration, and in the system deployment procedures. An important part of this research was to become familiar with the seismic system operation and to work with the Westinghouse Electric Corporation and MSHA personnel to modify and improve the system. To accomplish this we participated in the planning, execution, and data analysis for a number of seismic field tests. Several in-mine field tests were conducted. From these tests the capabilities of an in-mine seismic system were analyzed and specifications were made for designing an operational in-mine system. Several portions of the work done on this grant were covered in previous reports. In particular the capabilities or the presently operational surface based seismic location system has been thoroughly documented by Durkin and Greenfield (1981). Portions of the location procedures and effects of mine openings on seismic signals have also previously been published. These portions or the work will only be summarized in this final report.

Jan 1, 1982

By C. W. Huggins

The objective of this Bureau of Mines research was to compare the size distribution of respirable quartz collected at coal mines with that of several reference standards used to quantify quartz in coal mine dust samples. Particle size measurements were made on 23 samples and 4 ref-erence standards using a scanning electron microscope in the backscatter electron mode of operation, interfaced with an image analysis system. The Mine Safety and Health Administration provided the 23 respirable coal mine dust samples, which were collected at surface and underground coal mines in 7 States. The accumulated particle size measurements in-dicate three of the reference standards, minus 5-um Min-U-Sil, minus 5-um Supersil, and NBS 1878, would be preferred over the fourth, Silver Bond B, for quantitative quartz determinations in coal mine dusts by X-ray diffraction and infrared spectrometry.

Jan 1, 1985