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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 Ralph H. Whaite

To assist the anthracite industry obtain technical data on pneumatic packing, the Federal Bureau of Mines imported a pneumatic packing machine from Germany and installed it in a mine of a cooperating company in the Northern anthracite field of Pennsylvania. This report covers the second in a series of experiments in applying pneumatic packing for controlling strata movement (subsidence) above mine workings in the Pennsylvania anthracite region. The first experiment2/ was begun in January 1950, in a section of the mine where about 50 percent of the original coal remained in the form of pillars; since the company did not plan to mine the pillars in this particular area, pneumatic packing of the chamber voids was done for test purposes only. During this initial test the machine was operated on 204 shifts, and 652,400 cubic feet of breaker refuse material (22,834 tons) was packed into the voids of 16 chambers. The work was completed in December 1951.

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 J. 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 suitable chemically under present standards for producing metallurgical coke. (b) Which coals require special and more intensive treatment in preparation than is now practiced. (c) Which coals cannot be considered potential sources of metallurgical coke regardless of preparation. This report is one in a county series that describes the preparation characteristics of the coals of Mingo County, W. Va.

Jan 1, 1956

By J. R. Ruark

Because of the importance of oil-shale reserves the Bureau or Mines resumed research investigations in this field beginning in 1944. The Bureau early decided to build a Large-scale demonstration plant to accomplish the dual purpose of obtaining design data and to produce crude shale oil for refining studies. Two 40-ton-Capacity batch N-T-U (Nevada-Texas-Utah) retorts were completed for this purpose in 1947. After a preliminary operation, the plant was used to investigate process variables of air rate, recycle gas rate, and shale particle size and crude. Correlations obtained from these variables are presented in this report. Researchers concluded that recycle gas was not necessary for efficient operation of the process. Short comings of the batch method of processing the oil shale are pointed out in the report. Several periods of prolonged production operations were carried out. During these periods, the retorts were operated to produce as much crude oil per day as possible. The lifetime operation of the N-T-U retorts was divides into three periods, namely, preliminary operation, process variable study, and production operation. During the preliminary operation, 187 runs were made with a total of 7,596 tons of raw shale used to produce 3,688 barrels of crude shale oil. During the process variable study, 179 runs were made with a consumption of 7,494 tons of raw shale and a production of 4,218 barrels of crude shale oil. The production operation consisted of 554 runs in which 22,457 tons of raw shale was used to produce 12,359 barrels of crude shale ail. The overall total for the lifetime operation of the retorts consisted of 920 runs with a total consumption of 37,547 tons of raw shale and a production if 20,265 barrels of crude shale oil.

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 R. A. Hatch

The United States depends mainly on foreign imports, principally India, for an adequate supply of sheet mica suitable for its many uses in the electrical and electronics industries. Sheet mica has, in fact, played an indispensable role in developing these industries,4/ and, in turn, the products of these industries (radio, radar, electric motors, and many others) have become indispensable to the military forces. Because or these conditions, sheet mica in its better qualities long has been classified as a strategic and critical material, and from this stems the wide-spread interest in substitute materials of which synthetic mica is one potential type. The United States Departments of the Navy and the Army entered into a cooperative agreement with the Bureau of Mines in 1947 to study ways and means of synthe-sizing and growing mica crystals. This is one of a series of reports5/ that describe the results of this program.

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 W. T. Benson

Peacetime production of mercury in the United States is controlled by world mercury prices, with significant lags to be expected between price increases or decreases and resultant increased or decreased production. Twenty-four mercury-bearing mines and prospects in widely separated districts in western and central Nevada and one property on the Nevada-Oregon border were examined and sampled. The purpose of the project was to determine if some of the properties warranted more extensive exploration work to obtain information on possible reserves of commercial-and sub-commercial-grade ores. The investigation of mercury deposits in Nevada was sufficiently widespread and indicated several areas of interest in the State that merit further exploration work.

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 J. B. Gayle

Because economic and geographic factors have focused particular attention on the use of anthrafines in blends containing Lower Kittanning coal as the low-volatile component, samples from this particular bed were selected for experimentation whenever practical. Carbonizing tests were carried out in accordance with standard procedures, using the Tuscaloosa and sole-heated ovens. Most of the results are in general agreement with those reported by previous investigators. Specific findings are as follows: (1) The effectiveness of anthrafines in reducing coal expansion is such that even highly expanding, low-volatile coals can be carbonized safely with suitable additions of anthrafines and careful control of charge density. (2) Increases in coke size, resistance to shatter, and apparent specific gravity appear to be characteristic for additions up to approximately 15 percent to a fixed base blend. When anthracite of minus-48-mesh size was used and the proportion of low-volatile coal simultaneously increased, these indexes increased only slightly or remained substantially constant. (3) No increase in breeze formation was noted for additions in amounts up to 15 percent. (4) Abradability of coke was increased by additions of anthracite of No. 5 Buckwheat size, but it either decreased or remained sub¬stantially constant when the inert was ground to pass a 48-mesh screen.

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 Donald M. Hausen

Diamond-bit performance and cost data accumulated by the Bureau of Mines in core-drilling schists reveal significant trends of economic interest. Low-quality, small-size drill bort were the most economical. The percentage of core recovery, type and size of bit, and bit matrix are also correlated with bit performance and costs. Detailed analyses of the factors affecting diamond-bit performances and costs are assessed in the tables, graphs, and discussion.

Jan 1, 1956