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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 K. K. Kershner

The purpose of this investigation was to develop methods on a laboratory scale for recovering tin from metallurgical slime, Tin chlorides were volatilized using mixtures of hydrogen chloride and reducing gases, such as hydrogen, carbon monoxide, hydrogen sulfide, ethane, propane, and butane. Optimum conditions were found to be n mixture of 3:1 of hydrogen and hydrogen chloride at 475° C. Over 95 percent of the tin was volatilized as chlorides. Low temperatures and relatively rapid rates of reaction are distinct advantages of the chloride volatilization process. Research is being continued with various slimes and will be extended to tin ores, where the method offers interesting economic possibilities in comparison with current tin-smelting practice.

Jan 1, 1957

By Lex B. Golden

The purpose of this investigation was to evaluate the corrosion properties of certain alloys of titanium and to compare them with those of unalloyed titanium. Such information should make it possible to determine the desirability of substituting these alloys for commercially pure titanium in certain applications. Titanium-manganese, titanium-chromium-iron, and titanium-vanadium-iron alloys, with 2 types of unalloyed titanium, I consolidated by arc melting and the other by powder-metallurgy techniques, were included in the study. Tests were carried out in sulfuric, hydrochloric, phosphoric, nitric, and mixed acids and in chloride solutions. All solutions were saturated with air.

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

By N. A. Eilertsen

Among the numerous Low-grade manganese deposits in eastern Aroostook County, Maine, the Dudley deposit near Mapleton in the northern district is one of the few known to contain an appreciable tonnage averaging above 10 percent manganese. The ore body, consisting of stratified manganiferous hematitic shale, is over 5,000 feet long and ranges in width from 30 to 175 feet. The deposit was extensively explored during 1942-44 by the Manganese Ore Co., a subsidiary of M. A. Hanna Co. of Cleveland, Ohio. Data obtained from this work were made available to the State and Federal Geological Surveys for estimating ore reserves. An estimate by the Maine Geological Survey, using a 10-percent manganese cutoff and to a depth of 200 feet, shows 609,000 long tons of manganese metal in material averaging 12.6 percent manganese. By lowering the cutoff limit to 5 percent manganese, the estimate was increased to 919,000 long tons of metallic manga¬nese in material averaging, 10.4 percent manganese,

Jan 1, 1957

By P. M. Gruzensky

In view of some of the outstanding properties of chromium, considerable effort has been made in recent years to prepare the high-purity metal in ductile form. The object of this investigation was to obtain such metal by electrolysis of chromic acid solutions and to determine the conditions that yield optimum results. The apparatus is described, as well as the parameters that received consideration. Ion-exchange resins were employed to remove cation impurities from the electrolyte. Tensile specimens prepared from the electrodeposits by arc melting, press forging, swaging, and drawing, were ductile at room temperature. INTRODUCTION Metallic chromium displays an exceptionally high resistance to corrosion, oxidation, and wear at elevated temperatures. Although these properties are utilized to some extent when chromium is alloyed with other metals, such as in stainless steels, high-chromium alloys and pure chromium are not employed as engineering materials because of a serious lack of ductility and impact resistance at room temperature. Because high-chromium alloys appear promising as refractory metals for applications such as in gas turbines, much interest has been shown recently in the preparation of uniformly ductile chromium and in determining which factors contribute to its brittleness.

Jan 1, 1957

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 and describes the preparation characteristics of the coals of Logan County, W. Va. According to present-day standards for metallurgical coal, many believe that the sulfur content of the coal should not exceed 1.25 percent? Coal with more than this amount has been used for making metallurgical coke, especially when blended with coal containing less sulfur. In this series of reports 1.25 percent sulfur is used as a gage to determine whether or not a coal will be suited for metallurgical coke.

Jan 1, 1957

By J. B. Gayle

A 1/2-ton experimental coke oven was installed ac the Bureau of Mines Southern Experiment Station, Tuscaloosa, Ala., in 1948. Designated as the Tuscaloosa oven, this unit features a 17-inch carbonizing chamber, globar heating elements, and silica-brick walls designed to simulate as closely as possible the carbonizing conditions for commercial slot-type ovens. Because of the small force exerted on the oven walls in most tests conducted to date (probably owing to the practice of charging coals and blends at a moisture content approximating that normal to commercial plants operating in this district), little information has been obtained about expansion properties. Two sole-heated ovens have therefore been constructed and used as supplementary equipment for determining the expansion properties of coals tested in the Tuscaloosa oven. The reasons for constructing the Tuscaloosa oven, the details of design, the operating, characteristics of the oven and the reproducibility of results have been discussed in previous publications. 3 4 5/ The present report deals with the effects of substituting various high- and low-volatile coals for components of a selected base blend carbonized under conditions similar to those normally used for producing foundry coke. Results of tests of 11 coals and 14 blends indicate that several blends tested rave cokes having physical properties very similar to those produced from the reference blend.

Jan 1, 1957

By H. F. Yancey

The Baum-type jig used so widely to clean bituminous coals has not been adopted for anthracite. If proved suitable for anthracite, its use might lower preparation costs in some plants. Cleaning trials on a Pennsylvania anthracite in a laboratory-size Baum-type jig were undertaken by the Bureau of Mines to provide indicative information that would be helpful in determining whether the cost of a full-scale installation would be justified. Clean coal surpassing standard anthracite specifications was obtained in all sizes from Stove through No. 5 Buckwheat. Recovery effi¬ciencies were acceptable down to 3/16-inch size, but there was excessive loss of coal in the finer sizes. Thus the fine refuse produced in a commercial plant might re¬quire retreatment. A comparative cleaning trial in a dense-medium pilot plant provided a recovery efficiency only l percent higher than obtained in jigging.

Jan 1, 1957

By R. W. Huber

A consumable-electrode arc-melting furnace was constructed at the Bureau of Mines Physical Metallurgy Laboratory, College Park, Md., for the production of uncontaminated titanium and titanium-alloy ingots. The furnace was designed to allow for evacuating to very low pressures and back filling with helium and argon mixtures for melting at or near atmospheric pressure. Vacuum melting at a few millimeters pressure was also used with a mixture of helium and argon gas sweeping the crucible. For research purposes a 25- to 30-pound ingot, 4 inches in diameter by 15 inches in length, was selected to provide, enough 1/2-inch plate for extensive tensile and impact testing of standard size specimens. Enough plate was also provided for testing by other Government laboratories. The homogeneity of several alloy ingots was determined, and excellent results were obtained. By using a large electrode-to-ingot-area ratio and high currents or power inputs to the arc furnace rather uniform ingots were routinely prepared.

Jan 1, 1957

By D. E. Wolfson

As a part of its overall program of coal carbonization, the Bureau of Mines is studying the coking properties of coals that may be used for metallurgical purposes. The objectives of this study were given in detail in a previous report.2/ The inherent suitability of coal for metallurgical use depends primarily on (1) chemical composition, (2) preparation characteristics, and (3) carbonization behavior. The first two factors, as well as the available reserves, are considered in selecting coals for carbonization tests.

Jan 1, 1957

By J. R. Nettle

A method has been developed in the laboratory for successfully electro-refining titanium metal. Refining is accomplished in e fused-salt electrolyte using offgrade metal as the anode and collecting the purified metal at the cathode. The characteristics and requirements of the various alkali chlorides tested as electrolytes are discussed in relation to relative ease of purification and serviceability. The various types of cells designed and tested for electrorefining are illustrated and their method of operation discussed. The individual advantage of each cell and the purpose for which it was designed are reviewed. The magnitude of the cathode current density was found to depend largely upon the quantity of soluble titanium chloride in the electrolyte. The physical condition of the anode also greatly affected the cathode current density.

Jan 1, 1957

By Alla D. Mah

Titanium forms several compounds with oxygen and also is able to dissolve interstitially about 33 atomic percent of oxygen. Starting with titanium dioxide, reduction becomes increasingly difficult as oxygen is removed; and the final step, be reduction of the titanium-oxygen interstitial solutions, is by far the most difficult. The possibility of reducing titanium oxide, or of purifying titanium containing oxygen, by treatment with certain more volatile metals has been a subject of considerable interest. Theoretical appraisal of the limitations of this possibility, however, has been hampered by lack of adequate information on the thermodynamic properties of the titanium-oxygen solutions. The purpose of the present work was to remedy this difficulty by expanding the thermodynamic knowledge regarding these solutions. The experimental work involved three types of calorimetry and furnished the following information: (1) Heats of formation of 11 titanium-oxygen solutions, in the range of 0 to 10 wt.-percent oxygen, were determined at 298.15° K. As a byproduct, an improved value of the heat of formation of rutile was obtained, which, in turn, led to improved values of the heats of formation of the lower titanium-oxygen compounds. (2) Low-temperature heat-capacity data and entropies at 298.15°K in were determined for 2 representative titanium-oxygen interstitial solutions. (3) High-temperature heat-content data were obtained for 2 titanium-oxygen interstitial solutions to about 1,600° K.

Jan 1, 1957

By J. P. Powell

The importance of recovering more oil from known petroleum reserves has placed increasing emphasis on the application of secondary producing methods. One of the most successful of these has been the injection of water into depleted oil reservoirs. Water flooding is now recognized as a valuable conservation measure that not only prevents the premature abandonment of stripper leases but also is credited with reviving operations in many oil-producing areas previously abandoned. The injection of water into an oil-producing zone as a method of stimulating oil production was legalized in Kansas in 1935. Although water flooding had been attempted previously in other parts of the State, 1935 marked its introduction into the shallow stripper area of eastern Kansas. Two years later flooding was begun in the five-county area that is described in this report. Figure 1 is a map showing the water-flood areas in Allen, Bourbon, Crawford, Labette, and Neosho Counties, Kans. To July 1, 1955, the 77 projects in the oil fields of these 5 counties are credited with recovering an estimated 12.3 million barrels of oil that would not have been produced by methods used previously. These projects are expected ultimately to cover 10,700 acres, of which only 5,400 has been flooded to date.

Jan 1, 1957

By Clyde L. Brown

Recent developments in portable communication equipment for use in emergency recovery work following mine fires and explosions have wade possible a convenient and dependable means of directing rescue teams working under hazardous conditions. INTRODUCTION Mine rescue and recovery operations following; fires and explosions are frequently conducted under adverse conditions that require the use of oxygen breathing apparatus by members of a 5- or 6-man team. Conventional apparatus used for this purpose for many years was equipped with an oxygen supply adequate for at least 2 hours. The design of the apparatus is such that the nose passages are closed with a clamp, and breathing is accomplished through a mouthpiece connected to the apparatus by tubes and arranged to prevent inhaling air or gases from outside sources. The use of the mouthpiece has presented difficulties in the development of telephone communication because of the wearer's inability to speak while wearing the mouthpiece. The method of conducting operations of rescue teams requires a person to direct operations at a fresh-air base as close to the rescue team as possible. At least one standby rescue team and 2 or 3 other persons assigned to various tasks are stationed at the fresh-air base. An efficient and reliable means of communication between the director of operations and the rescue team is necessary for reasonably safe and efficient work in hazardous areas.

Jan 1, 1957

By Miro Mihelich

The mines and prospects in the vicinity of Landlocked Bay, 25 miles southwest of Valdez, Alaska (fig. 1), were examined, mapped, and sampled in July and August 1955 as part of a comprehensive investigation by the Bureau of Mines of ore deposits adjacent to Prince William Sound. The purpose of the investigation is to establish and record the location, nature, extent, and metallurgical characteristics of copper and associated metallization in the Prince William Sound district and to indicate, if possible, those areas in which additional exploration and development may be justified. Of particular interest are the possibly numerous deposits of massive iron sulfides that were neglected during early mining operations. These deposits may constitute important reserves of sulfur and iron. At Landlocked Bay deposits of copper-bearing iron sulfide minerals have been mined or partly explored through mine workings, which are in a zone about 1 mile wide along the western side of a large overthrust fault known as the Landlock Overthrust. Eight of the principal mines along this zone were examined end sampled. Although only three of the mines have a recorded production of shipping-grade copper ore, all have deposits of copper-bearing iron sulfide minerals that are similar in occurrence. The deposits occur as lenticular masses and disseminations of chalcopyrite, pyrite, and pyrrhotite which replace crushed rock or fill cavities along shear zones in greenstones and in sedimentary rocks that are exposed between sea level and an altitude of 2,500 feet. These lenticular masses of sulfide minerals range in size from small pods to ore bodies that have been stoped to maximum widths of 9 feet, strike lengths up to 70 feet, and dip lengths as much as 350 feet. Where accessible for sampling,, the copper content of the deposits ranged from a few hundredths of a percent to over S percent; zinc, gold, and silver are present in negligible amounts. Flotation tests of a sample composited to represent typical mine-run ore indicate that 81 percent of the copper is recoverable in a product assaying 28 percent copper at a concentration ratio of 17.5 : 1. INTRODUCTION Statistical records indicate that approximately 110,000 tons of metallic copper (about 16 percent of total Alaskan production) was produced from mines adjacent to Prince William Sound during the 40-year period ended in 1938. Although the principal production was from a large-scale mining and milling operation on Latouche Island (Kennecott Copper Corp., Beatson mine), a substantial amount of the total copper was derived from direct-shipping ores selectively mined or hand-sorted from numerous other deposits in the district. No production has been made since 1938; many of the claims have long been abandoned, and mine workings are either caved or deteriorating rapidly.

Jan 1, 1957