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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 Earl R. Maize

This is the first of a series of reports dealing with development of a method of strengthening bituminous-coal-mine roof. Later reports will describe the progress made with injecting high cohesive and adhesive bonding agents into bedding planes and mine tests of roof strata strengthened by the bonds formed. The concept of strengthening roof strata in coal mines by inserting steel rods in the form of bolts has been widely accepted by the coal industry. The benefits of increased production and safety derived from this type of roof support has more than justified the increased cost of roof bolting. However, not all coal-mine roof structure is amenable to this type of support, and failures occur owing to the heterogeneity and variable character of mine-roof strata.3/

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 W. J. Wenger

Colorado has been producing petroleum since 1863 but only recently has become a major oil State. The first well was drilled on Oil Creek near Florence, but out-put was relatively small until discovery and development of the Weber sandstone reservoir at Rangely. Oil was discovered in the Weber sandstone in 1933, and the reservoir was developed after 1940, bringing Colorado, in 1949, to 11th place among the 48 States as an oil producer. Colorado's output increased further because of the discovery and development of many fields in the Julesburg Basin since 1949 By 1954 Colorado was in ninth place and maintained that position through 1955.4/ Between 1946 and 1951, Colorado's oil production more than doubled, while the total United States production increased only 25 percent. It seems probable that production will continue to expand in Colorado for many years. This report presents analyses of 92 crude oils from 73 fields representing 90 percent of the production in 1955. Abridged analyses are listed for easy comparision, and complete analyses arc given in the appendix. Oil samples were collected for study from many different sources. Although many of the newer fields were not sampled, their oils probably are very similar to those from corresponding formations that were studied and tabulated.

Jan 1, 1957

By A. J. Barry

Five makes of expansion-type shells and two types of bolts (mild-steel and high-strength) were used in 30 tests made in sandstone and shale roof, The results show that the anchorage obtained in both the sandstone and shale were stronger than either type of bolt. That is, the yield loads of both bolt types were exceeded before excessive anchor slip occurred. A relationship for evaluating the anchorage effectiveness of 3/8-inch-diameter, expansion-type bolts is presented. A comparison of test results indicates that the anchorage effectiveness of 5/8-inch- and 3/4-inch-diameter expansion-type bolts did not differ appreciably.

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 R. R. Wells

This report summarizes the results of laboratory testing of copper-bearing magnetite ore from the Poorman, Bush & Brown, and Copper Center deposits, Kasaan Peninsula, Prince of Wales Island, southeastern Alaska. The ores contain minor amounts of chalcopyrite and pyrite. Intimate association of these sulfides with magnetite necessitates fine grinding for adequate liberation and rejection of copper and sulfur and for the production of high-grade iron concentrate low in objectionable impurities. Laboratory tests indicated that the optimum results can be obtained by flotation of ore ground to minus-100-mesh, with subsequent wet magnetic separation treatment of the flotation tailing. A summary of results obtained by this treatment of the three samples tested is shown in table 1.

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

By K. E. Stanfield

The Bureau of Mines oil-shale program, initiated in April 1944, is concerned with the future utilization of oil shale in the United States as a source of liquid fuel. One phase of this program is the accumulation of information on the location, extent, and richness of oil-shale deposits that may be suitable for processing to oil and related products. A previous publication5/ presented, by means of logs, the oil yields of sections of the largest known oil-shale deposit in this country -the shales of the Green River formation occurring in adjoining portions of the states of Colorado, Utah, and Wyoming. This present supplementary report presents the oil yields of cores from 48 holes drilled during 1952 to 1954 in the Green River formation of Colorado, which is distributed over an area of more than 1,000 square miles. The oil yields of the 48 oil-shale sections, involving the assay of 9,651 samples, representing 22,451 feet of core, are presented by means of logs. In addition, the oil yields of samples comprising the maximum sections of 15 gallon-per-ton shale are tabulated for these cores and for the 28 cores from Colorado which were logged in the previous report.

Jan 1, 1957

By J. B. Rosenbaum

This report presents new findings and consolidates previously published data to provide a single reference containing a concise and comprehensive description of the Bureau's work on electrolytic chromium. Two separate systems for electrolytic-chromium recovery were developed, one designated as the oxidized system the other as the reduced system. The electrowinning of chromium metal follows the dissolution of chromium from the ore or from ferrochrome and its separation from gangue and metallic impurities. Chromite was first solubilized by pressure digestion at slightly elevated temperatures in an oxidized acid solution using Na2Cr2O7 as an oxidizing agent. Later it was found that a sodium-free electrolyte was preferable, using return-cell anolyte containing H2SO4 and Cr03 as the oxidizing agent. Gangue materials were separated from the soluble metallics by filtration; and, after the Cr+3 had been stabilized, the metallic impurities were separated as crystalline ammonium salts by vacuum crystallization.

Jan 1, 1957

By F. N. Bender

Percolation leaching of wad-type manganese ores was investigated, using a novel system of alternate upward passage of sulfur dioxide gas through moistened ore and downward percolation of wash solutions to extract solubilized manganese. Bench and large-scale tests designed to simulate vat and heap leaching were made on four wad ores from Arizona and Nevada and on a pailomelane ore from Arizona. Three of the wad ores required prebaking at 500° to 600° C. to produce a permeable agglomerate that would not slake during percolation washing. The hard-type ore and one of the wad ores that contained a large amount of granular gangue did not require prior roasting. The deportment of the different ores toward leaching and percolation was studied with particular reference to the influence of the sulfur dioxide - oxygen ratio and the effect of gas dilution on the rate of manganese dissolution, dithionate formation, and acid production. Crushed charges of the ores, as coarse as 1 inch and as fine as 1/4 inch, were treated for periods of 5 to 11 days. Percolation of the gas and leach solutions through the charges was achieved without difficulty. The manganese extractions varied between 78 and 97 percent and depended upon the size and type of ore leached. The average quantity of sulfur dioxide required in the larger scale tests was about 2.6 pounds per pound of manganese recovered. The dithionate formation varied from 0.35 to 0.9 pound per pound of manganese extracted depending upon the strength of leaching gas.

Jan 1, 1957