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By G. R. Speich

RECENT studies by Smith and Olney,1,2 Olney,3 Greifer and Salli,4 Rys etal., and Olney and smith 6 have established that graphite is the first decomposition product to format the surface of hypereutectoid plain-carbon steels when they are austenitized in a vacuum or inert atmosphere and slowly cooled. This graphite evidently forms directly from the austenite and only at the surface of the specimen. The interior of the specimen is found to be free of graphite. The graphite layer can almost completely cover the specimen surface and the rate of its formation is markedly sensitive to the orientation of the austenite. The present work was undertaken to study this phenomenon further, especially with regard to the effect of temperature and austenite orientation. The material studied in this work was a high-purity iron-carbon alloy containing 0.88 pct C, 0.005 pct Mn, 0.016 pct Si, 0.005 pct S, and 0.002 pct P. Specimens were heat-treated in a commercial hot stage modified for rapid quenching.7 This permitted direct observation of the formation of the surface graphite. A vacuum of 10"" to 10-5 mm of Hg prevented oxidation or decarburization of the specimens. Specimens were austenitized for 30 min at 1100°C and quenched to a series of lower temperatures where they were isothermally transformed. Surface graphite was observed to form at 700°, 750°, and 780°C but not at 825°, 900° or 1000°C. Since the maximum solubility of austenite for graphite is 0.88 pct C at 800°C,8 surface graphite only forms at tem-

Jan 1, 1962

By C. M. Bartley

Fluorspar, in addition to its familiar uses as a metallurgical flux and as a source of the electrolyte for aluminum production, has become important as an essential raw material in the rapidly growing fluorine chemical industry. The unique ability of fluorine to react and form compounds with al-most all other chemicals has made it one of the important elements in modern chemistry. Research and development over the past thirty years have resulted in a current annual production of fluorine chemicals that is both technically and economically important to industry. Because many of these chemicals and products are relatively new, and most have properties that are not duplicated by other materials, the present uses are expanding rapidly and new applications are being reported continually. Fluorspar, the only immediate and practical source of fluorine, is therefore an important mineral. This fact has been recognized in major industrial areas such as the United States and Western Europe, but has received little attention in Canada.

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 Wilhelm in der Schmitten

A necessary condition for a uniaxial stress distribution in compression testing is that the specimen end surfaces make full contact with the apparatus compression plates. In addition all compression surfaces must be machined perpendicularly to the loading axis. In general this condition is not sufficiently fulfilled in a simple apparatus. Therefore on application of the load the compression plate may first touch the specimen at one point only. This may cause crumbling of the specimen if the material under investigation is brittle (e.g., ionic crystals). It also precludes a precise study of the beginning of deformation as the effective cross sectional area is unknown. In addition a complex stress state is set up which renders quantitative work impossible, e.g., on dislocation density and arrangement as a function of stress. To overcome these difficulties a "self-adjusting" upper compression plate is required. A simple and reliable method of achieving this is shown in Fig. 1: A steel hemisphere is placed on the specimen. As soon as the compression plate (which no longer needs precise machining) makes contact with this hemisphere the load is uniformly distributed over the whole specimen surface, and a homogeneous uniaxial state of stress results. An advantage of the method is that the loading is always central, even when the specimen surface is not parallel to the compression plate (Fig. 1, dashed line). Therefore to a first approximation a uniaxial state of stress is maintained if the misorientation of the specimen end surface is small. Two typical stress strain curves of identically prepared sodium chloride crystals are shown in Fig. 2; curve 1 was taken without and curve II with the hemisphere under otherwise identical conditions. The improvement in the accuracy of defining the beginning of elastic and plastic deformation is clearly indicated. The writer wishes to thank the Deutsche Forschungsgemeinschaft for financial support, and Professor P. Haasen for providing facilities for this work.

Jan 1, 1962

By K. C. Dean

A flotation method was developed by the Bureau of Mines for concentrating pollucite, a cesium-aluminum-silicate mineral that may contain from 20 to 40 percent cesium oxide. Separation of the pollucite from three typical ores was achieved by froth flotation of the associated micas, feldspars, and other gangue minerals, using sulfuric and hydrofluoric acids and a cationic-type collector. A low-tenor, 8 percent cesium ore from Maine was upgraded to 20 percent cesium with recovery of 87 percent of the cesium. Relatively high- grade ores from Canada and Southern Rhodesia were beneficiated at lower ratios of concentration to 28 and 29 percent cesium content respectively with recovery of over 92 percent of the cesium. In addition to concentrating the cesium content of ores, the method also effectively separates cesium from sodium, potassium, and lithium, and in certain ores from rubidium. This is accomplished by selective froth flotation of the alkali metal-bearing gangue minerals such as lepidolite, other micas, and feldspars. Since the alkali metals, especially potassium and rubidium, are difficult to separate chemically or thermally from cesium to prepare high- purity cesium products, separation by physical mans is important.

Jan 1, 1962

By B. H. Bergstrom, J. J. Gilvarry

Previously the authors showed that the Gilvarry equation correctly describes the distribution of fragment size in single fracture, provided the exoclastic particles showing original surface of the specimen are removed from the distribution. In the present work this conclusion has been strengthened in two respects. First, it has been shown that the existence of two peaks in the differential distribution for the endoclastic particles, corresponding to the effect of surface and volume flaws in the interior of the specimen, can be demonstrated from the average of data for a large number of specimens. Second, it has been shown by means of a Coulter counter that data obtained from specimens fractured in gelatin display the behavior at fragment sizes approaching 1 p which is demanded by the limiting form of the Gilvarry equation in this case. In previous work, a rigorous derivation of the proper distribution function for fragment size in single fracture of a brittle solid has been given by Gilvarry,' based on a closely defined physical model and deduced strictly by the laws of probability. Experimental work has been reported by Gilvarry and Berg-str~m,~ confirming the theory in its broad outlines. Subsequently, Gilvarry and Bergstrom extended the theoretical discussion to include comminution and presented experimental data bearing on this point. They have described further experimental results for the case of single fracture recently. The experimental evidence regarding single fracture was rather convincing. However, it was based on only five specimens for which fragment sizes were determined by sieve analyses and three for which measurements in the finer sizes were made on a Coulter counter. The purpose of the present paper is to extend the experimental results as obtained by means of both sieve analyses and the Coulter technique. In the former case, sufficient specimens are included so that the average data should vield ac- curately the detailed behavior of the distribution function for the coarser fragment sizes. In the latter case, measurements for the finer sizes are reported which correspond to single fracture more closely than prior results and fill a lacuna left in the experimental verification. In addition, an extension of the theory given recently bGilvarry for the case of fracture of a two-dimensional solid will be outlined, and experimental results obtained by him will be discussed.6 THREE-DIMENSIONAL CASE Gilvarry' has shown that the Schuhmann size modulus is a measure, in a sense specified later, of the number of activated edge flaws in a specimen undergoing single fracture. Single fracture is defined as that resulting from a single instantaneous application of energy, such as the blow of a hammer whose motion is halted when fracture begins. Plural fracture consists of a short sequence of single fractures, as in a jaw or gyratory crusher; multiple fracture obtains when many applications of energy are made, as in a ball mill. The Griffith flaws associated with fracture of a specimen are flaws occurring within the volume of the body, on the new surfaces created within its interior and on the new edges (intersections of two surfaces) within the body. Fracture proceeds by activation of flaws in the volume of the specimen, in the fracture surfaces throughout its interior, and in the edges produced by intersection of fracture surfaces. If all the flaws and all groups of flaws are distributed at random, independently of other flaws or groups thereof, it has been shown by Gilvarry that the distribution function for fragment size has the form of a Poisson distribution. The fraction y, by weight or volume, passing a sieve of mesh size x is given by where k is an average spacing of activated edge flaws, j2 is an average amount of surface containing one activated surface flaw and i3 is an average volume corresponding to an activated volume flaw. The averages in question are referred to the mean dimension x of a fragment. On the basis of the theoretical

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 T. V. Philip, R. E. Lenhart

When commercial silicon iron sheets of varying magnetic quality are isothermally annealed at high temperatures, extremely large grains develop in the material having good magnetic properties. These grains are of the (110) [001] orientation and are formed by secondary recrystallization. The primary driving force for this secondary recrystallization is grain boundary free energy. For the secondary grains, activation energies of 103 kcal per mole for nucleation, and of 75.5 kcal per mole for growth, were obtained. The activation energy for nucleation of the secondary grains is consistent with a model involving redistribution of a precipitate acting as the primary grain growth inhibitor. SINGLY oriented silicon iron sheet was first produced in 1935.1 The material as commercially produced today has a very highly developed preferred orientation or texture; up to 95 pct of the grains are crystallographically oriented with their (110) planes in the plane of the sheet and their [loo] directions parallel to the rolling direction. This texture, usually written as (110) [00l], is referred to as the "GOSS" or the "cube-on-edge" texture. Because the magnetic properties of this material are superior to those of the nonoriented sheets in the direction of rolling, the oriented silicon iron has acquired tremendous industrial importance especially in the manufacture of transformer cores and other electrical equipment. The commercially produced material is essentially an iron-silicon alloy containing about 3 1/4 pct Si with minor impurities totaling less than 0.15 pct. The silicon steel heat is melted in the open hearth or electric furnace. The ingots are hot rolled, with or without being slabbed, to strips of 0.100 to 0.080 in. thickness. They are then cold reduced to an intermediate thickness, recrystallized, cold reduced to final thickness, decarburized, and finally annealed at a high temperature. During this high-temperature anneal, extremely large grains with the cube-on-edge texture are produced in the sheet. Several papers have appeared in the literature2-10 relating to the production of the Goss-textured material. Most of these describe the textures produced on cold rolling and on subsequent annealing of single crystal or polycrystalline silicon iron. May and Turnbull11,12 have recently shown the necessity of a second-phase dispersed impurity in the material for the production of the Goss texture. However, none of these papers describes in detail the nucleation and growth kinetics of the (110) [001] grains during the final high-temperature anneal.* The present work, therefore, is an attempt to understand the nucleation and growth kinetics of the cube-on-edge grains in the silicon iron sheet during the final high-temperature anneal.

Jan 1, 1962

By J P. Bolduc, P. E. Pelletier

Preceded by brief general considerations such as the development of the mining industry in. the Province of Quebec, the choice of plant location, the types of problems studied etc., the paper gives a complete description of this new research and treatment center for metallic, non-metallic and asbestos ores. Facilities for carrying out operations in the three sections of the plant -the sampling section, the ore treatment section and the asbestos section -are fully discussed as well as laboratory facilities for (a) the preliminary testing of ores prior to pilot plant treatment and (b) the grading and testing of asbestos fibre. AT THE beginning of the century, the annual value of the mineral production of the Province of Quebec stood at the $2,500,000 level. Twenty-five years later, it was just under $24,000,000. In 1950, half a century later, it was slightly in excess of $200,000,000. But in 1959, in the span of only nine years, it

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 Robert S. Warfield

The Federal Bureau of mines and U.S. Geological Survey conducted exploratory investigations and geologic mapping in the Wishbone Hill district of the Matanuska coalfield almost continuously from 1942 through 1958. These investigations delineated reserves of high-volatile bituminous coal necessary to supply the rapidly expanding military and civilian requirements in the Anchorage area. This report describes the program conducted by the Bureau of Mines from 1949 through 1958, and briefly summarizes previous investigations, the results of which have already been published. The coal-bearing structure on both the north and south limbs of the prominent Wishbone Hill syncline was explored by 8,719 feet of churn drilling and 25,460 feet of diamond-core drilling. A total of 33 holes were drilled ranging in depth from 60 to 2,114 feet. To supplement the drilling operations, bulldozer and dragline trenching were undertaken at key locations; about 25,000 cubic yards of dragline trench were excavated in the vicinity of the old Premier mine.

Jan 1, 1962

By John C. Machisak

INJURY experience and employment data for the nonmetal mining industry in the United States are presented for the calendar year 1958. Statistical tables 6 to 12 give detailed information on injuries and employment at nonmetal mines. Data for nonmetal mines are presented separately from those for nonmetal mills, tables 23 29. The Bureau is authorized to send questionnaires to the nonmetal industry for their voluntary submission on of injury and employment experience at their operations. As this information contributes to the promotion of safety in the nonmetal mining industry, every effort has been made to make these questionnaires as complete as possible.

Jan 1, 1962

By George C. Branner

This circular is concerned with eight nonferrous scrap metals as they generated, collected, prepared, and consumed in California. Brief reference also is included with respect to Nevada and Hawaii. Four of these scrap metals - copper, lead, aluminum, and zinc - are of major importance and make up about 95 percent of the total value, whereas the remaining four - antimony, magnesium, nickel, and tin - make up the remaining 5 percent. For convenience, the subject matter is divided into three parts, (1) Data with respect to the collection, preparation, and marketing practices that are common activities to all the nonferrous scrap metals; (2) separate discussions and statistical data with respect to each of the eight nonferrous scrap metals in California; and (3) data with respect to Nevada and Hawaii.

Jan 1, 1962

By Martin H. Rogoff

This publication combines a critical review of the literature on the microbiology of coal with an introduction to those areas of microbiology related to studies of coal as a biological material. The attack on coal by microorganisms as yet remains doubtful. Only the low-rank coals contain an indigenous microbial flora, and even these organisms are not peculiar to coal, but are common soil and water forms. No experimental data have as yet been presented, either in the literature or in the present work, which unequivocally demonstrate the oxidation of coal by microorganisms. Reasons for the resistance of coal to such attack, including insolubility, physicochemical structure, steric hindrance of enzyme action, and the presence of antibiotic materials in coal are discussed. Microorganisms do attack large aromatic molecules and the mode of oxidation of aromatic ring systems by bacteria is presented. Well-defined pathways are known for the oxidation of polycyclic compounds with one to three rings, and these paths with their key intermediates are described and related to the possible oxidation of coal.

Jan 1, 1962

By F. G. Schwartz

This circular presents the results of a survey of research on jet fuel thermal stability jointly sponsored by the National Petroleum Refiners Association (NPRA), Tulsa, Okla., and the Bureau of Mines. The development of supersonic planes has led to many problems that did not exist in the operation of subsonic aircraft. One of the most important of these is rapid deterioration of the fuel at the high temperatures to which it is subjected. At higher speeds, aerodynamic heating of the airframe imposes severe thermal problems, and conventional techniques of rejecting the heat to the atmosphere become impractical. The fuel is the only material present in sufficient bulk to be used as a heat sink. Thus, the fuel is subjected to aerodynamic heating and also is used to dissipate heat from lubricating oil, hydraulic fluid, electronic equipment, wheel wells, and cabin air. Consequently, the fuels may have to withstand both moderate temperatures for sustained periods in the fuel tanks and higher temperatures for brief periods during transfer from the tanks to the combustion chamber. Because of high temperatures, insoluble residue or gum may form in the fuel and contribute to heat exchanger fouling and to clogging of the fuel manifolds, nozzles, control systems, and other components of the fuel system.

Jan 1, 1962

1. BOYD, JAMES. Statement on the Investigation of Natural Resources. Hearings before National Re-sources Economic Subcommittee, Committee on Public Lands, U.S. Senate, 80th Cong., 1st sess., on Investigation of the Factors Affecting Minerals, Fuels, Forestry, and Reclamation Projects, May 15, 16, and 20, 1947, pp. 125-131. 2. BUCH, J. W., HENDRICKS, T. A., AND TOENGES, A. L. Statement on the Investigation of Natural Resources. Hearings before National Resources Economic Sub-committee, Committee on Public Lands, U.S. Senate, 80th Cong., 1st sess., on Investigation of the Factors Affecting Minerals, Fuels, Forestry, and Reclamation Projects, May 15, 16, and 20, 1947, pp. 231-235. 3. CONGRESS, U.S. An Act to Provide for the Establishment and Operation of a Research Laboratory in the Pennsylvania Anthracite Region for Investigation of the Mining, Preparation, and Utilization of Anthracite, for the Development of New Uses and Markets, for Improvement of Health and Safety in Mining, and for a Comprehensive Study of the Region to Aid in the Solution of Its Economic Problems and to Make Its Natural and Human Resources of Maxi-mum Usefulness in the War Effort. Public, No. 812, 77th Cong., 2d sess. (S-357), ch. 764, approved Dec. IS, 1942, 2 pp.

Jan 1, 1962