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By Joseph A. DeCarlo

The rapid growth of the organic chemical industry in the United States and abroad has focused attention on the future raw-material sources for this important industry. Chemical products are essential to modern civilization; and millions of tons of organic chemicals are used annually, ranging from basic raw materials to finished chemical products such as drugs, cosmetics, and soaps. Hundreds of chemical products are made directly or indirectly from coal, but in this report "coal chemicals" will be limited to crude tar, crud light oil, and ammonia recovered in the high-temperature carbonization of bituminous coal and the important principal products obtained by processing these materials. Specifically these include benzene} toluene, xylene, naphthalene, creosote oil, tar acid oil, pitch, and ammonium sulfate. Therefore the term "coal chemicals", wherever used in this report, includes only these products and does not include the secondary or intermediate products such as styrene, synthetic phenol, aniline, phthalic anhydride, or finished products made from these, such as synthetic rubber, plastics, and dyes. The United States leads the world in production and consumption of coal chemicals. In the past five years nearly one-fourth of the total output of coal-tar crudes in the world was produced in the United States. Consumption of some of the more important products derived from these crudes such as benzene, toluene, xylene, and naphthalene, however, ranged from about one-third to one-half of the world total because of imports and production of benzene, toluene, and xylene from petroleum. The synthetic organic chemical industry of the United States was established during World War I on chemical raw materials obtained by the high-temperature carbonization of bituminous coal but this source of supply currently furnishes less than 40 percent. More than 60 percent of the chemical raw materials used to produce organic and inorganic chemical is supplied by the petroleum industry and production of petrochemicals is rising rapidly.

Jan 1, 1960

By W. E. Robinson

Oil-shale kerogen was processed into oil and oil products before the first oil well was completed by Drake in 1859. However, because of economic and other advantages, natural petroleum has been the principal source of liquid fuels and lubricants since 1859 and is a convenient root of many [organic] chemicals in common use today. In recent years the difference has narrowed between the cost of producing liquid fuels from well petroleum and other sources. This narrowing of cost difference has resulted both from the increased cost of finding new sources of petroleum in the United States and the experimental demonstration of lowered costs for synthetic liquid fuels by the Federal Bureau of Mines and by industry. Available petroleum resources of this country are being reduced and eventually may be inadequate to meet the demand. Alternate means of assuring an adequate supply of liquid fuels for this country include the development of processes for utilizing other carbonaceous materials such as oil shale and coal.

Jan 1, 1960

By J. M. Toguri, K. Grjotheim

It is known 1,2 that the equilibrium between titanium metal, TiCl2 , and TiCl3, in a solvent of molten metal chlorides, is influenced both by the total amount of dissolved titanium and by the type of solvent. Assuming that the trivalent titanium forms the complex ion Ti111 Cl4, the equilibrium reaction may be expressed by the following equation, (Me) TiIII cl4+ 1/2 Ti = 3/2 TiII cl2+ (Me) Cl The ideal ionic equilibrium constant for this reaction is, Where the N's are the molar ionic fractions in the equilibrium melt, and (Me) the different types of cations present in the equilibrium mixture. The following thermodynamic relation is derived between Kand the concentration of cations in the equilibrium melt, mix The N"S are the equivalent ionic fractions, and so forth are constants corresponding to the standard changes in free energy for reactions in melts where only the cation indicated is present, and f (y1) is a function of the activity coefficients in the equilibrium mixture. When this term vanishes, a simplified linear relationship between In Kideal and the concentration is obtained. The simplified relationship has been applied with satisfactory results to the experimental data of Mellgren and pie,' and Kreye and Kellogg.2 MANY existing methods for the production of light metals involve the reduction of their respective metal halides in the presence of salt melts composed of alkali or alkaline earth chlorides. In such a solution phase, the light-metal halide may undergo stepwise reduction from a higher, to a lower valence, and finally to a zero valent state. In this connection, the disproportionation equilibrium is of great interest. In the case where the higher valence is three and the lower valence is two, the disproportionation equilibrium may be written as follows, 3 Me11 = 2 Me111 + Me [I] If this equilibrium occurs in a salt melt containing a large excess of alkali chlorides, a typical ionic melt is obtained. It is then possible to formulate the cation equilibrium: 2 Me+h' + Me = 3 Me++ [II] Reaction [11] is analogous to a cation exchange reaction. It has been shown thermodynamically that the equilibrium constant for such a reaction in 2

Jan 1, 1960

By J. Gurland

THE microstructure of sintered carbides consists of particles of metal carbides, such as WC and TiC, embedded in a metallic binder which is usually a cobalt—or nickel-rich solid solution. One of the important factors influencing the strength of the alloys is the degree of dispersion of the carbide particles in the binder matrix. While it is generally accepted

Jan 1, 1960

By Lloyd Williams

A vertical air shaft in the Birmingham, Ala., iron district was sunk with a circular cross section and lined with concrete at a relatively low cost to provide needed ventilation for an iron-ore mine. The method of sinking the shaft is described, and the costs are stated in mar-hours with a descriptive list of equipment and a statement on the size and use of temporary buildings. Preparation began May 2, 1955, and the shaft was completed at a depth of [680] feet by September 22, 1956. By October 1956, all temporary building and [aft]-sinking equipment had been removed. The total direct-labor cost for the operation, including preparation and dismantling, was 50,700 man-hours, or 30.2 man-hours per foot. Total rock and dirt removed amounted to 17,523 cubic yards (in place), and the shaft lining required 4,635 cubic yards of concrete to form a circular air shaft with an inside diameter of 16 feet.

Jan 1, 1960

By E. C. Tarpley

The Federal Bureau of Mines has studied solvent extraction as a means of concentrating the mineral components in coal. Solubilities of a number of American coals were determined using abietic acid as a solvent. The effect of rank on solubility was investigated, and maximum solubility was found with coals of intermediate rank. Vitrinite is the most soluble petrographic component; fusinite, micrinitc, and exinite are nearly insoluble. Spore exines also have a low solubility. Abietic acid is a hydrogen donor and reduces pyrite to ferrous sulfide. Mild hydrogenation of high-molecular-weight fragments of the coal structure to those of lower molecular-weight probably contributes to the solvent action. Even where solubility of the coal substance exceeds 90 percent, contamination of the mineral matter with coal makes identification of the mineral components difficult. Further separation might be possible by the application of float and sink techniques to the residue. INTRODUCTION Work n the solvent extraction of coal is conducted to recover commercially useful products and to characterize coal;. and obtain information on their structure. Some coals, particularly those of low rank, contain waxes, resins, and humic acids which can be removed by solvent extraction and find varied industrial uses. In World War II, solvent extraction of coal was conducted on a commercial scale in Germany to obtain a low-ash feed material for hydrogenation and to produce electrodes carbon for the aluminum industry.4 5/

Jan 1, 1960

By H. L. Gibbs

Many factors contributed to the decision to build a radiochemical laboratory at the Salt Lake City Metallurgy Research Center to investigate the application of radioactive isotopes and chemical compounds in extractive metallurgy. These reasons included the notable success achieved in biological sciences with radioisotopes, the development of reliable instruments and methods for identifying the isotopes and measuring their activities, and the commercial availability of radioisotopes in a variety of forms and known activities. The paramount reason, however, was the realization that better methods were needed for guiding and quantifying research to resolve the complex extractive metallurgy problems under study at the Research Center. This is the first of a series of reports describing the application of radioisotopes and radioactivity techniques in extractive metallurgy. The report includes a discussion of licensing and safety requirements, a general description of the laboratory and the methods used, a definition of the nature and scope of the research program, and a synopsis of the more important problems studied. Subsequent reports will concern radioactive techniques for solving specific problems in mineral dressing, hydrometallurgy, and pyrometallurgy.

Jan 1, 1960

Strain-Hardening Exponent of Cross-Rolled Beryllium Sheet by S. R. Maloff, Vol. 215, No. 5, page 872, was omitted from Table of Contents for the October issue. Stabilization Phenomena in Beta Phase Au-Cd Alloys by Howard Birnbaum, Vol. 215, No. 5, page 786. The figure denoted Fig. 1 should be Fig. 3, Fig. 3 should be Fig. 4 and Fig. 4 should be Fig. 1. The captions are in the proper sequence. Activity of Carbon in Liquid Iron Alloys by Tasuku Fuwa and John Chipman, Vol. 215, No. 4, page 708. First equation, right hand column, page 710 should read

Jan 1, 1960

By Gill Montgomery

This report covers operations at the Crystal-Victory and Minerva No. 1 mines in Hardin County, Ill., which are operated by the Minerva Oil Co., Fluorspar Division, with offices in Eldorado. It describes the exploration, development, and mining practices, giving costs of each. Transportation, equipment, power, labor, and other influencing factors also are discussed. The mining methods employed are those most applicable to the flat-bedded replacement deposits common to the Cave-in-Rock section of the Southern Illinois fluorspar district. The fluorspar beds occur from surface exposures to 1,000 feet deep. In this district churn drilling is the method practiced for exploring flat-bedded deposits from the surface. Aerial photography and geochemical methods for indicating mineralization have been helpful in planning a drilling program. A program usually includes enough drilling to obtain only sufficient data on the value of the ore body and its structure to justify initial development and purchase of the mineral rights under option.

Jan 1, 1960

By W. A. Grosh

Records show that much of the lead produced in the Upper Mississippi Valley lead-zinc field was taken from natural openings along crevice systems at shallow horizons or at the surface. During the early history of the district, the shallow deposits were worked intensively; but in recent years the production of lead, except as a byproduct of deeper mining for zinc ores, has not been significant. Considering the methods of early mining, the character of mineralization, and the fact that galena can still be found on the surface of the old digging areas, it was reasoned that enough mineralization might remain on and above bedrock to permit, through the use of modern equipment and methods, economical re-treatment of surface material in the digging areas.

Jan 1, 1960

By G. Bridgstock, S. S. Forbes, E. M. Elkin

"OPERATIONS at Canadian Cop-per Refiners Limited, since the refinery was established in 1931, have been described in previous papers ( 1,2). Since then the refinery has treated the entire copper output of Noranda Mines Limited and Hudson Bay Mining & Smelting Company Limited. With the commencement of production in 1956 at Gaspe Copper Mines Limited, this copper has also been refined. From the start of operations to the end of 1958, the following had been refined: copper, silver, gold, selenium and tellurium.Construction of new buildings and additions to other buildings have been needed to handle increased receipts. The refining capacity has been increased from 112,000 tons of copper per year to a total of 236,000 tons per year.The refinery is located at Mont-real East, Quebec, close to railway and highway facilities. Incoming materials and shipments, with some small exceptions, are handled by rail. Some finished products are sl1ipped by industrial flatcar to the adjoining plants of Canada Wire & Cable Company Limited and Noranda Copper & Brass Limited."

Jan 1, 1960

By R. F. Tenney

The performances of four anthracite-burning stokers have been observed under identical 74-hp. steam boilers. Fifty runs of 12 and 24 hours' duration were made in accordance with the test code of the American Society of Mechanical Engineers (ASME). The capacity of each stoker for burning anthracite has been determined, the heat efficiency at each fuel rate has been computed, and the various significant items of hear loss have been estimated. The operating data and results from each run are tabulated in this report in the form used in the test code. The heat efficiencies and most significant operating data for each run are also presented graphically for each stoker to establish the trends with increasing boiler outputs, The tests show that rice anthracite can be burned on stokers adapted to its use at heat-conversion efficiencies of 82 percent or more under continuous firing. These high efficiencies are maintained with fuel inputs 30 percent higher and lower than the peak efficiency rate. Moreover, a heat efficiency of 70 percent or more is obtained at 50 percent of the optimum fuel rate, even though the excess air into the furnace cannot be held below 150 percent.

Jan 1, 1960

By H. Marshall Farrier

In the past few years the world petroleum industry has increasingly felt the weight of changes in the principal economic factors affecting pro¬fits. As a result of, these changes, it has been necessary for many oil companies to acquire certain new facilities in order to strengthen their competitive positions and thereby protect their tremendous investments in crude oil reserves, pipe line facilities, refining operations, and marketing outlets. Principally these needs have been met by new capital outlays. A supplementary, method of acquiring needed facilities, however, has been to obtain existing facilities through complete or partial acquisition of other companies.' properties. It is this method of meeting competitive pressures with which this paper is concerned. This paper presents a statistical breakdown of the mergers and acquisitions which occurred in the oil industry between January 1, 1954, and October 1, 1959, showing the frequency' with which certain types of properties were acquired in each of the years studied. In addition, it discusses the principal economic conditions which stimulated many of these property trans¬fers, comments on the effects of these mergers on the consuming public, and indicates the types of, mergers and the rate at which they may be expected during the next three or four years. The basic data upon which the statistical analysis presented in this paper is based were taken from several published sources. Obviously they are somewhat incomplete because not all mergers and acquisitions were reported However;, a careful search was conducted through, The Wall Street, Journal, The Oil and Gas Journal, Potroleum Week, and The Oil Daily with the result that the data should be reasonably complete and comparable for each of the years studied, It is believed, therefore, that the statistical analysis which' follows provides a reasonably accurate indication of the general trend in mergers and acquisitions during the period studied.

Jan 1, 1960

By W. A. Backofen, M. L. Ebner

SINCE the early work of Gough with Hanson and Wright,l-3 the study of fatigue has been characterized by experiments on single crystals only in recent times.9-10 Now, increasing attention is given to this aspect of fatigue research for the insight that it may provide into details of mechanism. The investigations have concentrated to a large extent on the development of deformation markings on fatigued crystals, and have shown the cracks to originate in slip bands possibly preceded or accompanied by slip-band extrusions. Experiments of special interest to the present work were conducted by paterson5 on copper crystals and involved both metallographic examination and measurement of change in flow stress. Crystals were cycled in alternating tens ion-compress ion with a constant plastic shear-strain amplitude of approximately 0.8 pct, and were particularly revealing for their demonstration of hardening with accumulated strain similar to that in unidirectional straining, through an easy-glide stage I followed by a stage II of rapid hardening; deformation was not continued beyond 40 cycles, however, so that the eventual course of the hardening curve could not be decided. For the conditions used by Paterson, surface slip markings were similar to those observed in unidirectional straining, but there were no X-ray asterisms and no deformation bands on the surface. In current thinking about the nature of fracture in fatigue, two views relative to mechanism are generally acknowledged, with the reservation that both could apply simultaneously in some measure. As one possibility, fracturing across a slip plane is regarded as a result of loss of cohesion from the creation of many point defects by dislocation movement under the cyclic loading.'' On the other hand, fracture has also been taken to follow as a consequence only of the geometry of slip at a free surface, consisting of offsets and crevices which eventually become fatigue cracks.12, l3 The work of McCammon and Rosenbergl4 showing fatigue in polycrystals at 4.2oK makes clear that any long-range diffusion of point defects is unnecessary, yet studies such as those of Forsyth and stubington15 show that accelerated diffusion may be a characteristic of deformation under fatigue loading. Interest in obtaining data of possible use for resolving such questions led to the experiments described below. Copper crystals were conveniently loaded in alternating four-point bending at constant deflection, a test condition shown to approximate a constant plastic strain amplitude for a wide range of axial orientations. The method of testing was not readily adapted to extensive study of temperature effects, but an investigation of the geometry of crack formation could simply be made by orienting,the slip direction at different angles to the surface. EXPERIMENTAL PROCEDURES Single crystals were grown by a modified Bridgman method in a stationary gradient furnace under an atmosphere of purified dry nitrogen. Purity of as-grown crystals was 99.999 pct as determined by spectrographic analysis plus vacuum fusion and gravimetric analyses for oxygen and sulfur, respectively. Crystals were of reasonable perfection as evidenced by a critical resolved shear stress at 10 deg from (110) of 60 g per sq mm and half-width of a (400) X-ray diffraction line from one crystal of

Jan 1, 1960

By J. L. Konchesky

The technical feasibility of gasifying powdered, noncoking, low-rank coal with steam in an externally heated tube has been demonstrated. The tube, 112 ft. of alloy-steel tubing shaped into a helix, served as an electrical conductor of electricity used for heating. The effects of the following variables were studied: Residence time of coal in reactor, average reaction temperature, steam concentration, and rank or geologic age of coal. Reaction pressure was maintained in the range 19-26 p.s.i.a. High carbon conversions and large yields of synthesis gas were obtained with low-rank coal. In one test, for example, about 88 pct. of the carbon in a subbituminous C coal was gasified at 1,910* F. with a residence time of 1 sec. The gas contained 58 pct. H2, 19 COD 15 CO, and 3 CH4; the yield was 30 cu. ft. (at 32' F. and 14.7 p.s.i.) of synthesis gas (CO + H2) per pound of dry coal.

Jan 1, 1960

By C. Stamberg, W. McGuire, R. C. Carlson, L. W. Vollmer

"The selection of materials and pre-cautionary measures for handling natural gas and condensate containing aqueous hydrogen sulphide are presented. Based on the results of a pilot production test and laboratory studies, together with several years . of operating experience, it was found that the behaviour of materials in sour gas environments can be predicted sufficiently accurately for engineering purposes.The selection of proper materials is essential for preventing sulphide-stress cracking. Where high strength materials are not required, low car-bon steel is used. Components requiring high tensile strength and hardness characteristics should be made from K-monel or properly heat-treated carbon-manganese-molybden-um and AISI 4140 steels. Welded connections are a potential source of sulphide-stress cracking. Consequently high quality welding and strict inspection are suggested as the most economical precautionary measures available.A maintenance program based,. where possible, on visual inspection of equipment and/or test spools located at strategic points should be used to follow weight loss and putting corrosion in sour gas environments. If severe weight loss or pitting corrosion is encountered, inhibitors have been found to be an effective deter-rent."

Jan 1, 1960

By John D. Grothe

Laboratory experiment as a basis of commercial plant design has been the subject of much analysis and thought and on which a large number of articles and papers have been published. We would be forced to choose between an unduly brief exposition if we wanted to cover it completely, or no exposition at all. We must therefore concentrate upon the essentials without ignoring at the same time too many of the qualifying factors which, by the choice of what we want to examine, may become side issues. In doing so, we do not imply that these side issues are therefore any the less important. In every case, what is said here applies with almost equal force to the pilot plant which may be necessary as it does to the commercial plant. In discussing a recent paper by Derek C. Shelton on the Santa. Barbara Mill in Chihuahua at a meeting of the Inst. of Mining & Metallurgy (London), D. J. Ottley said on the matter of relating laboratory results and small scale tests to full scale plant results that he would like' to draw the attention of members to the great difficulty of scaling up mineral dressing plants and processes. He felt that this was an important yet neglected subject which merited considerable fundamental scientific attention from mineral dressers and plant design engineers in particular. How much of this fundamental scientific attention has, as a matter of fact, been accorded to the subject, mainly by our sister profession, Chemical Engineering. The close similarity to chemical engineering problems that we meet, particularly in hydrometallurgical operations, suggests that Chemical Engineering publications offer a rich source of information and discussions of methods useful to us. We have only to think of pressure leaching, ion exchange, liquid-liquid extraction, precipitation and so on, all problems in chemical engineering unit processes or of the new Freeport Sulphur Nickel plant in Cuba or the Sherritt Gordon plant and many others.

Jan 1, 1960

By J. P. Capp

This experiment, one of a series on underground gasification of coal, was an investigation by the Federal Bureau of Mines of hydraulic fracturing as a means of increasing the air acceptance of a coalbed to permit introducing combustion air and removing product gases. Specific objectives of the investigation included: (1) Fracturing a coalbed; (2) determining the distance the coal was physically affected; (3) ascertaining the effect of the fracture on air acceptance of the coalbed; and (4) gasifying the coal. The coal was fractured with a fluid consisting of 15,000 lb. of sand mixed with 10,000 gal. of fuel oil and 5,000 gal. of kerosine, injected at pressures up to 900 p.s.i.g. and rates up to 425 g.p.m. The oil served as the fracturing medium, and the sand as a propping agent to hold the fracture open. From the fracture point, (the place in the bed where the fluid was injected), the fracture extended 200 ft. or more along the face cleats, somewhat less along the butt. cleats, and was confined to the coalbed. At the fracture point, the bed accepted about 500 std. c.f.m. of air, which was an etghtyfold increase. Fracture effects were extensive, as airflow was noted from old mine workings and outcrops 600 to 800 ft. from the fracture point. It is probable the actual fracture was much less than 600 ft. and that normal coalbed permeability beyond the fracture limits was responsible for this flow. This indicated that effects of the fracture extended beyond the area of coal physically affected. Although no attempt was made to gasify coal more than 200 ft. away, these effects plus the natural permeability of the bed likely would permit combustion beyond the outer limit of the fracture. As these experiments continued for more than 2 years, and greater air acceptance due to the fracture was observed at the beginning of each test, it is apparent that the effects of the fracturing persist for a considerable time.

Jan 1, 1960

By Henry H. Ginsberg

The effectiveness of 0.01 pct. molybdenum, as ammonium molybdate impregnated on coal, on the hydrogenation of a high-volatile bituminous C coal at 8,000 p.s.i.g. and 460° to 480° C. has been studied in a pilot plant by the Federal Bureau of Mines. Under these conditions, the Bureau obtained 98 to 99 pct. conversion5/ of coal to liquids and gases at throughputs of 29 to 101 lb. of m.a.f. coal per cubic foot of reaction space per hour. At 460° C. the indicated yield of oil ranged from 63 pct. (based on m.a.f. coal) at a throughput of 35 lb./c.f.h. (pounds per cubic foot per hour) to 68.5 pct. at a throughput of 58 lb./c.f.h., and the yield of gaseous hydro-carbons ranged from 25.5 to 19 pct. at the same throughputs. The maximum measured yield of oil boiling under 325° C. was 47 pct.

Jan 1, 1960

By H. E. Powell

A laboratory mineral-dressing investigation was conducted by the Federal Bureau of Mines on four limonitic and four sideritic iron ores from the North Basin of the east Texas iron-ore district. The samples, composited from drill cores, were considered representative of the iron-ore reserves of the area. The objectives of this research were twofold: (1) To devise a mineral-dressing method whereby the yield from currently mined east Texas iron ores might be increased and the grade improved, and (2) to extend such treatment to include the lower grade ferruginous materials that are not amenable to beneficiation by simple washing and, therefore, are not being exploited. Of the mineral-dressing methods used in this investigation, magnetic separation of roasted are was shown to be the most effective. Results show that, by this method, a laboratory recovery of 82 percent of the iron is attainable at a grade surpassing that obtained by current plant practice and that both limonite and siderite are amenable to concentration by the process. The existence of large deposits of iron are in eastern Texas has been recognized for over 100 years. These ores were first exploited during the Civil War and were mined intermittently until about 1911. From that time until 1944 when the Defense Plant Corporation financed the erection of three blast furnaces to use these east Texas ores, production was almost at a standstill.4/

Jan 1, 1960