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By D. E. Wolfson

As part of its overall program of coal-carbonization research, the Bureau of Mines is studying the coking properties of coals from various fields of this country. Few of the coals included in this survey are used for the manufacture of metallurgical coke, although some well-known coking coals necessarily are tested to provide comparative data, particularly on blending properties. The overall objectives of the study were given in detail in a previous report.3/ The inherent suitability of coal for metallurgical purposes, as distinguished from economic considerations, depends primarily on (1) the available reserves, (2) chemical composition, (3) preparation characteristics, and (4) carbonization behavior. These items are considered in selecting coal for carbonization tests.

Jan 1, 1956

By M. L. Skow

Large tonnages of the manganese ores found in Aroostook County, Maine, are refractory to conventional mineral-dressing techniques and to the common chemical- extraction procedures. The Maple Mountain-Hovey Mountain ores are typical of this type. Because the most promising method of recovering the manganese from these ores has been a chloridizing roast in which the ground ore is in contact with gaseous hydrogen chloride, preliminary batch tests were made with a fluidized bed. On the basis of these tests, it was concluded that fluidization, with careful control of operating conditions, could be employed for this cloridization and warrants further study. Selective volatilization of the iron at 600° C. was unsuccessful. An operating temperature of approximately 950° C. was necessary for a practicable rate of volatilization of manganese chloride. Hydrogen chloride contents of 10 to 100 percent of the fluidized gas gave essentially equivalent manganese recoveries with an 80- minute retention time, For shorter periods reaction was more complete with the higher hydrogen chloride concentrations. At the 80-minute retention period the lower hydrogen chloride concentrations volatilized somewhat less iron and also improved the physical operation of the process. Fluidization gave results superior to comparable tests on chloridization in a fixed bed.

Jan 1, 1956

By J. S. Browning

The purpose of this Bureau of Mines project was to develop a method for recovering kyanite and sillimanite from the present zircon-mill tailing of the Jacksonville and Starke, Fla., plants of Humphreys Gold Corp. The kyanite and sillimanite in the ore are not being exploited at present, but procedures for recovering the two minerals were worked out by the Bureau in the interest of conserving natural resources. The current zircon-mill tailing of the Starke plant contains up to 20 percent of a mixture of kyanite and sillimanite. A similar product of the Jacksonville plant contains up to 15 percent kyanite and sillimanite. The average annual production of the tailing now being stockpiled contains several thousand tons of the two minerals. Laboratory batch-flotation tests were made on the materials to determine the feasibility of flotation methods for recovering high-grade concentrates. Various reagents were employed under different conditions to determine the optimum conditions for flotation of kyanite and sillimanite and retardation of the gangue materials. The results of the preliminary flotation tests were encouraging enough to warrant more comprehensive testing of a larger sample of the ore in the laboratory pilot plant.

Jan 1, 1956

By F. E. Block

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

Jan 1, 1956

By John B. Gayle

The suitability of fluid petroleum coke as a blending agent for producing metallurgical coke has been investigated using the Tuscaloosa and sole-heated experimental ovens. From the results of tests with three representative blends, it has been fond that additions of fluid petroleum coke effect the following changes: (1) Increase in size, resistance to shatter, and apparent specific gravity of cokes produced; (2) little or no change in coke hardness and stability or in the amount of breeze formed; (3) increased charge density; (4) modification of expansion characteristics of blends charged; and (5) decreased ash and increased sulfur contents of blends charged and cokes produced. Substitution of a calcined sample of fluid coke of greatly reduced sulfur content resulted in a coke of inferior physical properties. This effect indicates that additions of the calcined product should probably be limited and that other methods for producing a low sulfur fluid coke should be considered.

Jan 1, 1956

By Manuel Gomez

A lignite from Milam County, Tex., has been oxidized by air at temperatures from about 27° to 300° C. for varying lengths of time. The oxidized coal was carbonized at 500° C. in a laboratory assay unit, and the products of carbonization were measured and analyzed. The data presented suggest that, as lignite is progressively oxidized, tar yields are decreased and gas yields are increased in a ratio approximating 1:1. It is surmised that tar-yielding structures in the nonoxidized coal produce gas, principally, when the coal is oxidized. Char-yielding structures of the nonoxidized coal give rise to additional water of decomposition after oxidation and pyrolysis. As lignite is subjected to greater oxidation, the gaseous product evolved on pyrolysis becomes almost entirely carbon dioxide. Tar yields decrease with an increased degree of oxidation, so that the reduction in tar yield may be used as a qualitative measure of oxidation. Pilot-plant drying and carbonization, where air is used as the transport gas and where some air is included in the drying and carbonizing gases, induces some oxidation of the coal particle. The short residence time in a fluidized system with reference to the oxidation environment limits the oxidation.

Jan 1, 1956

By F. W. Wessel

This report summarizes Bureau of Mines laboratory tests of four tungsten¬-bearing materials of various grades, The test work has demonstrated that the dry reaction between sodium carbonate and scheelite is best conducted at 900° C. or a few degrees less. The sodium carbonate requirement, in addition to the stoichiometric equivalent of the scheelite, is in some inverse relationship to the grade of tungsten in the ore. Residence time and particle size exert a definite but minor control on the reaction. Pressure-digestion tests on an impure concentrate indicate the technical feasibility of extraction by this process. INTRDUCTION Over 100 years ago Oxland discovered that tungstic oxide could be removed from wolframite and converted to a soluble form by reacting the mineral with a soluble alkaline salt at elevated temperatures. He patented this discovery, and this patent 4/ since has been the basis for most tungsten extraction. Much literature exists on this process and its modifications, and the characteristics and possibilities of the reaction are quite well defined.

Jan 1, 1956

By R. T. MacMillan

Many bench-scale tests and studies have been conducted in developing and testing a chloride-volatilization procedure Ear treating low-grade manganese ore from the Maple Mountain-Hovey Mountain deposit of Aroostook County, Maine. The ore, averaging 10 to 12 percent Mn, contains manganese in several forms and is resistant to concentration or extraction by usual physical and chemical procedures. Over 90 percent of the manganese, content of the ore has been recovered using a chloridizing roast in which the ore was heated at 950°-9b0' C. in a circulating stream of hydrochloric acid gas. Chlorides of manganese and iron were volatilized and swept to a fume collector, where they were condensed and separated from the [as] stream. Operation of a small, 1-pound-per-hour shaft Furnace produced enough chlorides for studying other factors in an integrated process such as: (1) Conversion of the chlorides to oxides; (2) recovery of HC1 gas of suitable concentration Ear recycling to the chloridizer; and (3) control of the Mn-Fe ratio in the oxide product to produce a suitable feed for ferromanganese production.

Jan 1, 1956

By J. M. Riley

A fluorometric method using morin in an alkaline-buffered chelating solution has been developed by the Bureau of Mines for determining beryllium in ores and mill products. Apparatus for measuring fluorescence intensities of the beryllium-morin reaction is described. Preparation of the sample for analysis consists essentially of digestion with sulfuric, nitric, and hydrofluoric acids, fusion of the residue with sodium carbonate and sodium borate, Solution of the melt with sulfuric acid, and proper dilution. Chemical separation of other ions is usually unnecessary. The method rave reliable beryllium determinations on samples in the 0.01- to 0.37-percent BeO range. The method is particularly applicable to low-grade beryllium ores; however, semiquantitative beryllium determinations have been made on beryl containing 12.0 percent BeO.

Jan 1, 1956

By M. H. Salsbury

This report describes the tunneling at the Leadville drainage tunnel, which was resumed in September 1950 with funds made available in the 1950 appropriation of the Department of the Interior. It brings up to date the account of the first project, carried on from December 1943 to August 1945, published by the Bureau of Mines which supervised both the first and second projects. In this report Leadville mining history, particularly related to drainage efforts, and the possibilities for future mine drainage are discussed briefly. An account of the second project, including a description of the operating cycle, exploratory drilling done as a safety measure, surveying procedures, geology, cost data, and other pertinent information, completes the report.

Jan 1, 1956

By C. S. Allbright

This report gives the results of analyzing three groups of crude shale oils by the Bureau of Mines procedure:4/ (1) Oils produced by standard Fischer assay determinations on oil shales from Brazil (Paraiba Valley) and the United States (Colorado); (2) oils produced from Brazilian shale by different retorting methods; and (3) oils from high-temperature retorting of Colorado oil shale in the Entrained Solids retort. It is the second in a series presenting data obtained by analyzing crude shale oils from various sources. The series furnishes information on the general characteristics and compositions of a wide variety of shale oils. Use of a standard analytical method on all samples facilitates comparison of different oils. The 18 oil samples analyzed in this project comprised 3 from assays of Brazilian and Colorado oil shales in the Fischer retort, 9 obtained by processing Brazilian shale in various other units, and 6 from entrained solids retorting of Colorado shale at 1,000° to 1,500° F. The crude oils from Brazilian shale contained about half as much nitrogen as the Colorado oils. Properties of the Fischer assay oils from Colorado shales agreed with some data that relate grade of the oil shale with properties of the crude oil from the Fischer assay. Comparison of results from Fischer assays of oils from the foreign and domestic shales shows that the oil from Brazilian shale contains more low-boiling material and less residuum than either of the two from Colorado shale. This fact is reflected in lower specific gravity, viscosity, and carbon-residue values for the Brazilian oil. Retorting Brazilian shale in the Entrained Solids unit at 1,120° F. produced an oil whose boiling range was generally lower than the boiling ranges of oils obtained by processing in three other retorts at conventional temperatures. The quality of crude oils from high-temperature retorting of Colorado shale in the Entrained Solids process varies with retorting temperature. As the temperature is raised within the range 1,000° to 1,500° F., the amount of the naphtha fraction in the crude oil increases to about 35 percent and the aromaticity to 98 percent.

Jan 1, 1956

By R. W. Stahl

Methane, a highly explosive gas evolved during the coal-formation process, is one of the hazards of mining most difficult to overcome. It is retained between particles of coal and entrapped in strata overlying and underlying the coal beds to a degree dependent upon the permeability of the enclosing strata. Considering that methane might be encountered at any time during the mining of coal, attempts have been made through the years to minimize the sources of ignition at coal-mine faces, such as the introduction of permissible electric equipment, the prohibition of smoking and open lights, and the development of safer explosives. The sparks created when mining-machine picks contact sandstone or iron pyrites2/ constitute one source of ignition, always recognized as a possibility but never greatly emphasized in the United States until recently, when ignitions began occurring with rather alarming frequency and in widely scattered coal-producing areas.

Jan 1, 1956

By B. P. Martinez

In response to a request from the President, the Department of the Interior joined with other agencies in a comprehensive study of the land and water resources of the New England-New York region. As part of this study, chemical engineers of the Bureau of Mines have visited 1,025 mineral-industries plants to inventory the waterborne wastes of mineral origin, discharged by the mineral industries of the New England-New York region. Four-hundred and sixty-two of these plants disposed their wastes to a public sewer of some type, but waste control remains a problem for moat of them. The 1,025 plants are discussed in main industry groups according to their production: Chemical and allied products. Stone, clay, and glass products. Iron and steel and their products (except machinery). Nonferrous metals and their products. Electrical machinery. Machinery (except electrical). Transportation equipment. Miscellaneous mineral industries.

Jan 1, 1956

By John C. Hartley

Large areas of the anthracite beds in the Wilkes-Barre, Pa., region have been first-mined in such a manner that over half of the original coal has been left underground as pillars to support the overburden. To recover the maximum amount of this remaining coal, improved devices to support the roof while pillars are being extracted are needed. Also needed are suitable backfilling systems that will stabilize the strata during the mining and effectively limit the inevitable subsidence after pillars are removed. Accordingly, the Federal Bureau of Mines furnished 400 yielding steel props that had been purchased abroad, where this type of prop had been used successfully. The cooperating company arranged for concurrent tests with a mechanical stower designed and built by an American manufacturer. In the area in which the experiments were conducted, pillar removal, using conventional timbering, was most difficult because the roof fractured badly, the installation of timbers consumed a substantial part of the work effort, and some coal nearly always was lost. With the application of the yielding props, the time needed for securing the roof was reduced 33.9 percent; production per man-shift was in¬creased over 33 percent; coal recovery was improved more than 9 percent; and the convergence between roof and floor, during mining and backfilling, amounted to as much as 8.03 inches without any break in the roof. However, in September 1953 some roof rock fell in pillar 10 owing to insufficient props in a small area where the ends of three top holes drilled in the coal face extended up into the roof rock.

Jan 1, 1956

By H. R. Shell

Of three known compounds in the ternary system K20 - PbO - SiO2, one having the composition K2Pb4Si8021 crystallizes into a structure with asbestiform properties. This compound, whose silicon-oxygen ratio is between that of the layer silicates (for example, mica) and the double-chain amphiboles, crystallizes in the tetragonal system. It malts, apparently congruently, at 779° C. The fiberized product prepared from crystals is fluffy and closely resembles natural asbestos in appearance, but is more brittle and has less strength. However, potassium-lead silicate may be separated into fibers with a uniform diameter of 200-300 A.U., and the fibers show with the electron microscope the s criteria that have been interpreted as indicating a hollow tube structure in chrysotile asbestos. Since very few inorganic crystalline compounds have such a structure, the material has unusual scientific interest. Microcrystalline potassium-lead silicate was rapidly and completely formed when powdered glass of the same composition was heated to 650° - 700° C, but macrocrystals grew only slowly from the viscous massive glass. Maximum growth rate was 0.12mm. per hour at 700° C.

Jan 1, 1957

By B. C. Parks

This is the first of a series of reports on the relation between microscopic composition and chemical and physical properties of banded bituminous coals. It describes the relation between microscopic composition and behavior during thermal decomposition of a heterogeneous, high-volatile A bituminous coal from the Chilton bed in West Virginia. The standard free-swelling test was used as a simple means of studying the effect of heat on the coal. Although swelling indexes are not precise indicators of coal behavior in the coke oven and have limited value in caking investigations, they are reliable for predicting expansion of coal in a fuel bed and have practical value in the study of fuels. The swelling test also supplements other useful laboratory tests for determining the plastic and expansion properties of coal.

Jan 1, 1957

By B. W. Naugle

Twenty-nine sole-heated-oven expansion teats were made on 9 different coals, and apparent specific-Brevity tests were made on 12 of the resultant cokes. The coals, which ranged in dry, mineral-matter-free fixed-carbon content from 58.7 to 81.1 percent, were tested over a rather wide range of moisture content and dry-coal bulk density to determine the separate effects of these variables on linear coal expansion. The experimental data support the follow expression relating "as-tested" coal bulk density, moisture content, and linear expansion, [ER = (1-MR) (1+Et) - 1; BDt] where ER = fractional expansion at a reference bulk density of 55.0 lb. of 1 percent moisture coal per cu. ft., Et = fractional expansion at Mt and BDt, MR = reference moisture content = 0.01, Mt = moisture content, "as-tested", BDR = reference bulk density = 55.0 lb. per cu, ft., BDt = bulk density, "as-tested", 1b. per cu. ft.

Jan 1, 1957

By W. H. Oppelt

A small, annular-retort gasifier having a nominal capacity of 40 pounds of lignite per hour was designed and constructed at the Lignite Experiment Station, Grand Forks, N. Dak. The purpose of the investigation was to increase the capacity of an annular-retort gasifier by better temperature distribution in the heating chamber (adjacent to the annulus) and by supplemental internal heating with controlled amounts of air. Correct control of air admission should yield crude ammonia-synthesis gas having a (H2+CO)-N2 ratio of 3. Dakota Star stoker-size lignite was used during the exploratory experimental program. The effects of temperature level and distribution in the heating chamber and of addition of air to the reactor were investigated. Hydrogen - carbon monoxide ratios ranged from 1.9 to 2.5, and (H2+C0)-N2 ratios were as low as 2.9. Hourly gas production ranged from 970 to 2,580 cu. ft., or 62.0 to 164 cu. ft. per sq. ft. of heated surface, or 350 to 940 cu. ft. per cu. ft. of reactor volume. Data from the small gasifier could be readily correlated with those previously obtained in the commercial-scale unit under comparable experimental conditions.

Jan 1, 1957

By Joseph Berman

The wolframite mineral series was studied to determine the effect of the FeO - MnO ratio on unit cell symmetry and thermal stability. This work was undertaken to evaluate the analytical procedures now in use for wolframite in scheelite and to aid in the development of improved methods of analysis. Wolframite grains were hand-picked, crushed, and screened; impurities were removed by selective magnetic separations using a Frantz isodynamic separator. The samples were further checked by optical spectroscopic and microscopic examination.

Jan 1, 1957

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