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By J. G. Haymes

This report by the Bureau of Mines is the first of two proposed papers on evaluation of spectrophotometric, spectrographic, polarographic, and other analytical methods for quantitatively determining impurities in high-purity tungsten. Some of the methods described are standard methods that have been successfully applied to determine low-level impurities, several are modifications of known methods, and some procedures are entirely original. The Bureau of Mines is actively engaged in tungsten research because tungsten has an extremely high melting point, in fact the highest of any known metal. The metallurgist must know the content of impurities in tungsten because of the marked effects even micro amounts of impurity elements have on its physical properties. The Bureau procured a number of analyzed samples of above-average purity from research laboratories of companies engaged in production and fabrication of tungsten. These samples were investigated by the analytical procedures of those companies for several metallic impurities. Subsequent analytical laboratory determination of impurities in these samples agreed with the analyses as reported. With this assurance that analytical methods were basically accurate for metallic impurities, procedures for the determination of several of these elements were modified to lower the limits of detection and increase the sensitivity of methods. Carbon and the gases hydrogen, nitrogen, and oxygen were determined by standard instrumental methods, modified to provide greater sensitivity for reliable determinations when content of these elements was low. After the reliability of the modified procedures was affirmed, they were used as a product evaluation guide in the development of a vapor-plating technique for the production of high-purity tungsten. The following list of elements can be determined by one or more of these methods: AI, B, Be, Ca, Co, Cr, Cu, Fe, Mg, Mn, Mo, Ni, Pb, S1, Sn, Ti, V, and Zn. In addition, a vacuum-fusion method for the determination of H, N, and 0, and a conductometric method for carbon are described. Lower limits of determination and detection for each element listed are given.

Jan 1, 1962

By R. W. Stahl

An emergency is defined as an unforeseen combination of circumstances that calls for immediate action. When applied to a coal mine, an emergency may call for prompt removal of the men to the surface through travelways other than the haulageway or intake airways, which are generally contaminated with irrespirable air as a result of an explosion or fire. Therefore, maintenance of adequate and travelable escapeways from all working areas of a mine is vitally important insurance against disaster. Several mine disasters could have been avoided if well-defined escape routes had been provided and made known to all mine employees. Such occurrences, unnecessary as they generally are, unfairly indict the industry when only a small segment thereof is involved. As a result of a rather recent disaster, which might not have happened if good escape routes had been provided, the Bureau of Mines decided to delve into the escape procedure to determine (1) what is being done in the industry and (2) what might be done at reasonable cost.

Jan 1, 1962

By John D. Bardill

Data from extensive tests was obtained on friction-head losses of various sand slurries, composed of materials of different specific gravities and under varying transport conditions, to provide useful information for designing hydraulic transport systems. The tests were run in a pilot plant through 2-, 3-, and 4-inch lines with slurries composed of relatively pure barite and limestone solids. Available grinding and classification equipment did not permit attaining a comparable size distribution in the two materials tested, thus preventing direct correlation of friction-head loss values to physical properties or mineral composition. A total of 495 measurements were made of limestone slurries in the 2-, 3-, and 4-inch pipe test sections at flow velocities from 6 to 14 feet per second and pulp densities from 40 to 70 percent solids. A total of 640 measurements of barite slurries were made in the 3-and 4-inch pipe test sections at flow velocities between 7 and 14 f.p.s. and pulp densities ranging from 40 to 80 percent solids.

Jan 1, 1962

By V. F. Swanson

As part of the Bureau of Mines titanium resources examination program, samples of altered rock (saprolite) and unaltered rock from the Roseland anorthosite near Roseland, Nelson County, Va., were tested for amenability to beneficiation by flotation. A flotation technique was developed to produce bulk concentrates of ilmenite, rutile, sphene, and leucoxene. It was necessary to first float apatite using oleic acid as the collector, in an alkaline pulp with dextrine as a titanium mineral depressant. The titanium minerals could then be floated from the apatite tailing, using fluosilicic acid to depress the remaining apatite, morin to depress ferromagnesian minerals (when present), and oleic acid as the collector. A bulk titanium mineral concentrate, analyzing 66.0 percent Ti02 and 0.08 percent P205, was obtained from a sample of the unaltered rock which contained 5.45 percent TiO2 and 2.81 percent P205. Overall recovery in the concentrate was 47.1 percent of the total TiO2 in the ore. About 55 to 65 percent of the saprolite sample was clay and was removed by attrition scrubbing and decantation. The apatite prefloat procedure was applied to the saprolite sands; subsequent titanium mine: 1 flotation recovered 72.2 percent of the Ti02 in a bulk concentrate containing 65.1 percent TiO2 and 0.20 percent P205.

Jan 1, 1962

By H. D. Mellom

The direction of the optic or "C" axis of a uniaxial metal crystal can be found with the metallurgical polarizing microscope by examining two planes of section on the crystal. Complete orientation of the crystal can be determined if a twin crystal is common to both surfaces of section. Examination of Uniaxial Metals in Polarized Light-Rotation of a uniaxial crystal surface, properly prepared,' shows four extinction positions 90 deg apart, provided that the surface is not close to a basal section. One of these two extinction directions corresponds with the projection of the optic axis on the surface of section. This direction can be found if the 'sign of the rotationr2 for the metal is known. To find the direction of the optic axis, the crystal is rotated on the stage 45 deg from an extinction position. With a crystal of negative sign, to produce extinction the analyser must be rotated towards the optic axial direction and vice versa. All sections, other than basal, of a uniaxial crystal have the same sign of rotation and, since there is no change in sign with wave length, white light can be used for these measurements. U the sign of the rotation is not known the presumed direction of the optic axis can be determined assuming a positive sign. A third section cut normal to the presumed optic axis will show basal extinction if the assumption is correct. It is convenient to use the edge between the two planes of section as a fiducial direction common to both surfaces. The optic axis can be related to this direction. If the above measurements are repeated on the other plane of section and the angle between the two section planes measured, stereographic projection can be used to determine the orientation of the crystal optic axis. Determination of Complete Orientation—The complete orientation of a uniaxial crystal can be determined provided that a twin crystal is common to both surfaces of section, and the twin law is known. The orientation of the twin crystal optic axis can be determined in the same way as for the main crystal

Jan 1, 1962

Air tabling of zircon-rich non-conductor products containing quartz enables most of the fine quartz present to be rejected without a markedloss of zircon. The coarser quartz in the air table feed can be separated from the zircon by screening one or more air table products, the oversize products containing most of the quartz and little of the zircon. Air tabling, with or without screening, is more efficient than wet tabling alone for the removal of fine quartz, but not for the removal of coarse quartz. Practically all of the quartz can be separated from the zircon by using wet tabling in conjunction with hydraulic classification, or by using air tabling in conjunction with dry launder treatment, in which a degree of sizing takes place that is advantageous for subsequent air tabling.INTRODUCTIONBack-dune and inland beach sand deposits usually contain fine wind-blown quartz, and neither spiral nor wet table concentration, alone or in conjunction, makes a clean separation of heavy minerals from quartz. Many rutile plants recover rutile and zircon from a low-quartz, wet-table concentrates by means of magnetic and electrostatic separation; some rutile and zircon are lost in the table tailings. Other rutile plants, and two of the ilmenite plants in Western Australia, recover rutile or ilmenite respectively, from a spiral concentrate containing several per cent of quartz, and then subject the non-conductor product to an additionalgravity concentration process to separate the zircon from the quartz. Some zircon is lost in the additional gravity process, but all of the rutile or ilmenite in the spiral concentrate is, or should be, recovered as high-grade concentrate. The higher recovery of rutile or ilmenite by this treatment method is offset by the expense of drying part of the feed twice, as a wet process is usually used to separate the quartz...

Jan 1, 1962

Important factors in dredge design are the estimation of total head, and the determination of flow in and around suction nozzles and in pipe lines. Total head for the dredge pump is calculated from velocity, static, and friction heads. Flow into suction nozzles depends on whether hydraulic jets or mechanical cutters are used, and on nozzle shape. Design of pipe lines depends on the transportation characteristics of the pulp, skin friction, swirl, and the avoidance of cavitation. Measurement and control of flow is important.INTRODUCTIONEconomic deposits of heavy minerals along the east coast of Australia occur in frontal dunes, which are normally unconsolidated and granular, or in hind dune areas which may contain indurated seams interspersed with loose material. In working frontal dunes, dredging depths are usually shallow since values do not persist for more than a few feet below sea level. However, the controlling factor in dredging the hind dune areas is the level of the water table and suction dredges may be designed to mine to depths of 120 ft, or even more, if necessary.In previous applications of suction dredges in the industry attention was directed primarily towards production and there was only limited research on fundamental techniques. However, with lower grade deposits now forming the major ore reserves, production levels and profit margins will fall unless more efficient dredges are developed.For satisfactory design of dredges it is essential that the total head be accurately estimated and that detailed information of the principles of flow in and around suction nozzles be determined. This paper presents information gained from field experience and laboratory investigation on these aspects.

Jan 1, 1962

By J. B. Gayle

Commercial flotation plants operate on a continuous basis that is not simulated closely by the batch testing methods widely used in Bureau of Mines laboratory studies of flotation, Batch methods indicate whether a particular separation is possible but provide little or no information about the rates at which such separations can be effected in continuous operation, Therefore, laboratory equipment suitable for testing on a continuous basis was assembled for an investigation of a number of the operating variables that influence the flotation of coal. The results of these tests lead to the following conclusions: 1. Flotation recoveries were markedly influenced by variations in the percent solids in the feed, However, the relation between these variables is complex and depends on the particular coal and operating conditions used. Flotation rates generally increased with increased cell concentrations.

Jan 1, 1962

By Charles W. Huggins

A study of the high magnification of some inorganic fibers which are found in nature or produced in the laboratory, has been conducted with the electron microscope. This series of electron microqraphs shows the important morphological differences exhibited by potassium-lead silicate, lead-aluminum silicate, chrysotile, wollastonite, silicon nitride, potassium titanate, cobalt chrysotile, magnesio-fluor-richterite, fluor-richterite, refractory oxide fiber, silicon carbide, massive serpentine, and palygorskite. A ribbon or a thin lath 250-2500 A. wide is the structural form of potassium-lead silicate and lead-aluminum silicate. Chrysotile, cobalt chrysotile, and massive serpentine all have a tubular structure and a fairly uniform (150-300 A.) diameter. Wollastonite, potassium titanate, fluor-richterite, and magnesio-richterite crystals have a lath shape, and potassium titanate laths are laminated ribbons. Single fibers of silicon nitride and palygorskite are ribbons, and the silicon nitride sample contains many twins (branching fibers). Palyqorskite fibers are highly flexible and have cross-sectional measurements of 150-300 A. Silicon carbide fibers differ from other fibers because their structure consists of several different forms. The sample used in this study had, predominately, a margarite-type structure. The refractory oxide fiber lost, all its apparent fibrosity after being prepared for electron microscopic examination, and only irregular fragments are visible in the electron micrographs.

Jan 1, 1962

This report is the 25th in a series summarizing Bureau of Mines research and technologic work on coal and related investigations, and the 7th of these reports to be issued on a calendar-year basis.3 It reviews briefly work in progress during 1960, and furnishes references to publications by Bureau personnel during 1960 and also to a few older papers that were not cited in prior reports of this series. Details about some of the researches mentioned can be found by referring to the publications cited in the footnotes or in the further list in the Miscellaneous section; other phases of work are reported here for the first time and will be covered in more detail by later publications, Coal programs of the Bureau of Mines extend over the wide range of theoretical and applied studies indicated by the table of contents. Fundamental research on coal structure and on the properties of coal will, over a period of time, increase the general knowledge about coal Which scientists and engineers may use in answering practical questions and in solving problems in the mining and utilization of coal. More applied studies are conducted in connection with the developement and evaluation of new mining techniques and the effective processing and utilization of coal and of coal products. Health and safety activities, analyses of coal being mined, and technical advice and assistance to Federal agencies in connection with fuel and boiler-water problems are among the practical services handled by the Bureau.4 5

Jan 1, 1962

By Howard W. Wainwright

This bibliography was compiled by the Bureau of Mines as part of an investigation into the possible utilization of low-temperature coal-tar bases. The bibliography consists of literature and patent references from about 1945 to 1961 and is divided into the following headings: Analysis and Composition; Production, Synthesis, Reactions, and Utilization; and Separation, Purification, and Properties. Although over 1,000 references are included, no attempt was made to insure a comprehensive survey. The literature and patent references are arranged alphabetically by author or patentee. When several publications have the same author they are listed in reverse order of age, with the newest first. An author index is included because secondary authors are not cross-indexed. In almost every instance, the entry is accompanied by a Chemical Abstracts reference for those interested in locating an abstract of the original paper.

Jan 1, 1962

By Clarence Karr

THE BUREAU OF MINES is investigating methods for upgrading tar produced by the low-temperature carbonization of bituminous coal. This survey was undertaken to compile information needed for identifying the ether constituents of low-temperature tar. Physical properties are listed for 1,024 aromatic ethers. The compounds include cyclic and noncyclic, polyfunctional and monofunctional ethers with oxygen joined directly to either one or two aromatic rings. Alkyl groups up through butyl are included. The compounds are divided into 37 groups ranging in complexity from alkoxybenzenes to dibenzopyrans. Compounds containing aromatic ether groups are important constituents of the neutral oxygen components of low-temperature tar. For example, at Morgantown, W. Va., the Bureau of Mines has identified and determined the amounts of benzofuran, 2-, 3-, 5-, 6-, and 7 -methylbenzofuran, diphenyl ether, dibenzofuran, 2,3-dimethyldibenzofuran, and two other dimethyl-dibenzofurans in the neutral oil from a low-temperature bituminous coal tar (103, 104).3

Jan 1, 1962

By F. Fraas

ELECTROSTATIC methods are used to separate and concentrate or purify granular particles derived from ores or various synthetic and agricultural products. Compared with other separation methods that require many technological refinements, the electrostatic attraction of fibers, grass, and seeds to charged surfaces clan be accomplished under the most primitive circumstances, and the early development of this method of beneficiation seemed very promising. Precise application of the method to provide high selectivity, however, is a complex procedure, and interest in this method declined. During this period Mr. O. C. Ralston initiated a Bureau of Mines research program oil electrostatic separation. It is the purpose of thins publication to describe the development of the electrostatic method of particle separation from the early beginning to the present resurgence of interest. Most of the information for this description bas been derived from references, a few of which were not available for thorough review. Much information has been drawn from the investitions of the Bureau. Acknowledgments Mr. O. C. Ralston, former Chief metallurgist of the Bureau of Mines, began the research program on the subject and did research on the mils literature. Both Mr. Ralston and Mr. H. B. Johnson, former president of the Huff Electrostatic Separator Co., furnished patent references. A critical review by Mr. F. D. Lamb, Research director, and Mr. M. J. Spendlove, Supervisory metallurgist, Bureau of Mines, College Park Metallurgy Research Center, lifts been of much value in preparing this report.

Jan 1, 1962

By W. A. Krivsky, R. Schuhmann

Jan 1, 1962

By Sara Jane Boles

In recent years the interest in rare-earth compounds as refractory materials has exceeded the available literature on the subject. While some basic properties, such as density and melting point, of the more readily available rare-earth compounds have been reported in the literature, relatively few papers can be found that deal comprehensively and primarily with high-temperature refractory properties and applications of rare-earth oxides, carbides, sulfides, and nitrides. Therefore, this bibliography has been pre-pared for the use of the ceramic industry as a guide for locating and utilizing the scattered and frequently fragmentary information available. The term "rare earths", as applied in the literature search for this bibliography, is understood to include the following elements: cerium, dysprosium, erbium, europium, gadolinium, holmium, lanthanum, lutetium, neodymium, praseodymium, samarium, terbium, thorium, thulium, uranium, and ytterbium. (On the periodic chart, these elements appear as numbers 57 through 60, 62 through 71, 90, and 92.) It is emphasized that many of the abstracts included are from papers in which the rare-earth compound or compounds are treated along with several other ceramic materials, are mentioned only secondarily, with primary interest placed on a more commonly used refractory material, or are used as part of a mixture of materials formed experimentally and reported on in the paper. As the better known rare-earth materials, such as the oxides of uranium, thorium, and cerium, appear more frequently in the literature, they also appear more frequently in this collection. Articles abstracted include only information on the basic properties that are of interest to the refractories investigator. References to crystal lattices and related topics are generally excluded from this publication. The temperature 1,500° C. has been set arbitrarily as the lower limit for reported data on thermal properties. However, because of the scarcity of information, some reports are included in which data are limited to those obtained at lower temperatures. Many of the articles abstracted include lists of references that will be of additional assistance in pursuing specific lines of investigation.

Jan 1, 1962

By Paul Meadows

This Bureau of Mines report presents operating practices and results of pressure maintenance and secondary recovery by water injection or by water injection supplemented by gas injection. Particular emphasis is placed on the results of water injection, which is the principal oil-recovery method employed in projects covered by this report. No attempt is made to study gas-injection projects or operations that are considered water-disposal projects. Also, this report does not include water-injection projects that have not been in operation long enough to evaluate results. Figure 1 is a map of north Louisiana showing the geographical locations of the projects included in this report. Most of the data used in this study were supplied by unit operators, operating companies, and the Louisiana Department of Conservation. Reservoir information and recovery data are generally those supplied by the operators, but include revisions where deemed necessary.

Jan 1, 1962

By Joseph H. Bilbrey

COBALT is a silvery gray metal which closely resembles nickel in appearance and properties although it is somewhat harder and more brittle. It is rather widely disseminated and is estimated to make up about 0.001 percent of the earth's crust as compared to 0.020 percent for nickel. Cobalt, one of the four ferromagnetic elements, is used for many magnetic applications. It is oxidation resistant, a property which when coupled with its moderately high melting point of 1,495° C., makes it useful in high-temperature applications. Although cobalt had been used by man as a coloring agent for glass and other ceramic products for 4,000 years, it was not isolated as a metal until 1742 and not established as an element until some 40 years later. Early in the 20th century, cobalt began to be used in alloys, and soon these applications displaced ceramics as the major consumer of cobalt. The use of cobalt in alloys gave considerable stimulus to production, and the world output of cobalt increased rapidly, rising from 400 tons in 1920 to 1,400 tons in 1930 and 5,500 tons in 1940. With the advent of the jet plane in the mid 1940's and the consequent increased need for cobalt-bearing high-temperature alloys, cobalt production again increased, reaching 7,900 tons in 1950. The increased demand for cobalt during the Korean war coupled with a large demand for stockpiling caused world production to more than double within the next 10 years, reaching a peak of 17,300 tons in 1959.

Jan 1, 1962

By William R. Barton

COLUMBIUM (niobium) and tantalum are similar refractory metals with closely related properties and uses and close association in ore deposits. Until recently both metals, particularly columbium, were essentially laboratory curiosities. However, since the beginning of World War II, applied technology, under the impetus of national security requirements, has realized many chemical, electronic, nucleonic, and missile and rocketry applications, where high temperature or corrosive environments require the use of columbium or tantalum. At the same time, advances in these fields have resulted in intensive research on the geological distribution, resources, metallurgy, and properties of these two metals; their alloys and compounds; and the development of a full-fledged columbium-tantalum industry. The future appears to promise continued acceleration in such studies and ever-increasing demand for these elements. The raw material supplies of columbium are abundant, and the extractive metallurgy of columbium is well enough advanced to assure adequate supplies of the element at reasonable prices to meet any projected demands. Although the extractive metallurgy of tantalum is similarly well developed, raw material supplies are so limited that, lacking new ore discoveries, an increase in demand to five times the 1959 level would severely tax ore-production facilities. Approximately 120 tons of tantalum and about one-half as much columbium was produced in 1959. Additional quantities are consumed as compounds or additive alloys such as ferrocolumbium and ferrotantalum columbium (55).3

Jan 1, 1962

By G. D. Bakulev

Economic Importance of Gasification of Fuel and Brief Outline of Development of Underground Gasification of Coal in the U.S.S.R. The underground gasification of fuel offers a number of economic and social advantages, principally the following: 1. Full automation of labor-consuming coal-mining processes, which resist complex mechanization and automation, particularly shaft mining. 2. Elimination of hard, dangerous, and often unhealthful mining work. 3. Creation of hygienic conditions for personnel employed in gas production, as well as for those in boiler rooms using the gas. 4. Possibility of automation of complex production processes of thermal-electric powerplants using underground gas with economic installations for steam production. 5. Economic operation of thermal-electric powerplants constructed in the areas of underground-gas production. 6. Release of railroads from the burden of transporting fuel. 7. Extension of the power base of some areas in need of fuel and of the economy as a whole due to use of fuel deposits not amenable to normal mining practices. 8. Reduction of capital investments per unit of energy produced in the form of fuel. 9. Substantial increase in general labor productivity. 10. Possibility of substantial reduction in the cost of fuel produced and of electric power produced from underground gas.

Jan 1, 1962

By W. H. Tomlinson

This publication presents the basic text for a 20-hour accident-prevention training course developed for supervisors by the Federal Bureau of Mines. During the past 2 years, the course has been used by the Bureau in teaching more than 300 groups of coal-mine supervisors-men whose responsibility is twofold: To manage in production and maintenance phases of coal mining and to guide their men along paths of safety. This is a handbook for teaching teachers. In this handbook will be found references to safety practices followed by companies that consistently have low accident records. These companies credit their outstanding performance to the adoption and faithful observance of accident prevention by supervisors and workers alike on a wholesome, cooperative basis. Teaching safety to workers involves both on-the-job and classroom-type instruction. If such training is to be permanently effective, it must be reinforced consistently on the job by the immediate supervisor of the worker. This publication is intended to provide such a supervisor with the motivation to provide such follow-up and shows how he can accomplish it effectively.

Jan 1, 1962