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By Larry D. Patts

Section 317(e) of the Federal Coal Mine Health & Safety Act of 1969 directed the Secretary of the Interior to prepare standards under which all working places in a mine shall be illuminated by permissible lighting while persons are working in such places. Section 317(e) further provides that such working places shall be illuminated within 18 months after such standards are promulgated. In accordance with this section of the Act, there was published in the Federal Register for December 31, 1970, a notice of proposed rulemaking which prescribed the illumination to be provided in the working places of underground coal mines. In light of written comments, suggestions, and objections to this proposed rulemaking, the proposed standards were withdrawn and reproposed in the Federal Register for Wednesday, October 27, 1971. In light of further comments, suggestions, and objections, a public hearing was held on April 4, 1974, and standards were again reproposed and published in the Federal Register for April 1, 1976. Promulgation of the final lighting-standards &k place on October 1, 1976, which means that the underground coal mining, industry must comply with face illumination requirements by April 1, 1978.

Jan 3, 1978

By Chester N. Truax

Still another shadow was cast over coal's largest market-the electric utilities-when President Johnson signed into law the Federal Clean Air Act of 1967. Air pollution-sulfur reduction-was thus brought into sharper focus as one of the central problems of the coal industry. Industry executives testified in both Houses of Congress to enable the lawmakers to develop a workable and economic law. The new legislation calls for the Secretary of Health, Education and Welfare to establish air control regions. After the regions are outlined the Department will publish air quality criteria on pollutants. Anticipating this legislation, the coal and utility industries have for the last several years been involved in extensive research programs to develop solutions to the air pollution problem. Even though the coal industry has been under strong attack for its part in adding contaminants to the atmosphere, it is by no means the major contributor.

Jan 2, 1968

By Elton A. Youngberg

J. H. HEARDING, Jr.*—Extremely hard ferruginous chert (taconite) was encountered in driving a drift at the Fraser underground mine near Chisholm, Minn., on the Mesabi Iron Range. In order to get better results in drilling in this ground, it was decided to try tungsten carbide bits. In the beginning, 1½ in. tungsten carbide bits and 1 1/8 in. round-lugged alloy steel drill rods with "jack-stud" inserts were used. Considerable difficulty was encountered because the jack-stud became loose in the drill rods. Because there was not enough alloy steel drill rod on hand, we began to insert jack-studs in the ordinary high carbon drill rods and found, to our surprise, that there was less trouble with jack-studs working loose in these rods than there had been with the alloy steel rods. As a result, use of the alloy steel rods has been discontinued entirely. Under the heading "Drilling Procedures" the statement is made that all holes are started with detachable bits or conventional steel to prevent undue strain on the tungsten carbide bit inserts when collaring a hole on uneven ground. This practice was followed in our work originally for the same reason. It was soon found, however, that the holes could be started with the tungsten carbide without injuring the inserts if the drill operator was careful and did not give the drill too much air until the bit had a chance to seat itself in the rock. J. C. FRANZ*—In a discussion of other technical papers with reference to percussion drills and the use of carbide tungsten bits, it was my impression that the authors reported one of the first difficulties experienced with the use of standard, conventional percussion drills, was insert bit failures due to crushing of the bit inserts when the bits became dull. During the past few years, some of the rock drill manufacturers, I am told, have adopted an air drill for use with the carbide bits that have a lighter blow and faster rotation than the regular machine. This machine has been tested and the carbide bit failures have been considerably reduced. L. W. DUPUY†—The difficulties Mr. Youngberg mentions that were had with rod and coupling breakage call to mind similar troubles experienced at the Picacho mine in California near Yuma.6 The commercial couplings then available were found to be tempered almost to brittleness. Rod breakage was usually in the threads near the end of the rod. The highly-tempered couplings would break as soon as the rod broke. The solution was to thoroughly anneal the couplings and to put in only a very mild temper. Subsequently the alloy used in making the couplings was changed from the original by the manufacturer, but still only a very mild temper was used. The result was that the softer coupling would give but would not snap and release its hold on the broken rod thread. Fishing jobs were reduced to the few where the rods broke at the rod end of the thread. Thread breakage on the rods was further reduced by thorough annealing prior to tempering. The data Mr. Youngberg presents regarding the use of carbide inserts on long blasthole drilling is most interesting and it would appear that the use in this manner of percussion drills and carbide bits will have many applications. W. M. WOODWARD*—How many feet of hole, on the average, do you get from a tungsten carbide bit, and is there much variation from this average? E. A. YOUNGBERG (author's reply) —In recent months the 2 in. tungsten carbide bit footages in long hole drilling hake varied from 115 .to 140 ft monthly. The footages obtained from individual bits vary from several feet to over 300 ft, however the life of a majority of the bits will be within 25 ft of the average.

Jan 1, 1950

By Monte J. Pool, Rudolph Speiser, George R. St. Pierre, William T. Ebihara

Standard free energies of formation of WO,, W O W20058 and WO3from oxygen and the lower oxide or tungsten have been determined in the tempel-ature range of 700° to 1220°C. A tentative W-O phase diagmm is presented based on the evidence that the oxide phases, "W18O49" and "W20058", are unstable at l~atm total pressure, below 585° and 485°C:, respectively. A HE need for a complete quantitative treatment of the phase equilibria of the W-O system has been establishedby metallurgists during the past few years. In an attempt to improve the endurance of tungsten exposed to oxidizing atmospheres at high temperatures, many research groups have studied the kinetics of tungsten oxidation. The reverse process, the reduction of the tungsten oxides to metal, has also been investigated to some extent. Regardless of the particular interest, metal to oxide or oxide to metal, a knowledge of the phase equilibria of the W-O system is required to properly interpret all of the kinetic observations. It should be possible to state the stable phases of the W-O system at any given values of the chemical potential of oxygen and the temperature.

Jan 1, 1962

By Charles Waidner

IN response to many urgent requests for a concrete realization of a series of standard temperatures that would be available to any one anywhere for the standardization of pyrometers and the reproduction of the standard scale of temperature for use in laboratories and industrial works, the Bureau, in 1916, made arrangements with several manufacturers to prepare a series of- pure metals that could best serve this purpose. After the necessary preliminary work of chemical analysis, as a check on the purity, together with exact determinations of melting or freezing points, the Bureau began, in 1917, the issuing of melting -point standards of tin, zinc, aluminum, and copper. At the outset, it was decided to secure metals of the highest purity and of American manufacture, and this was accomplished in a more satisfactory manner than anticipated. In the preparation of these temperature standards, the Bureau has had the hearty cooperation of several American companies, which have succeeded in producing metals highly satisfactory for the purpose and of as high a state of purity as could have been obtained anywhere. Each company that undertook the responsibility of furnishing a metal for this series of standards exercised most painstaking care to produce the best possible product as to purity and uniformity. A representative of the Bureau witnessed the actual preparation of each metal. The 300 and 400-lb. (136 and 181-kg.) samples making up the first series were all used up, with the exception of the aluminum, early in 1919. The Bureau has taken steps to replenish its stocks of metals serving as pyrometric standards and to the list has been added lead. The copper and lead are being ordered this time in 1-ton lots and the zinc and tin in 300-lb. (136 kg.) lots as before. The wide dissemination of these samples will be appreciated when it is noted that the metals are distributed by the Bureau inn quantities of 50 cu. cm. each, at $2 a sample and accompanied by a certificate which gives the melting point as determined by samples from the same lot. The manufacture and detailed description of chemical analyses, physical measurements, and precautions in use of these pyrometric standards, are described in detail in the Bureau Circulcar No., 66.

Jan 8, 1919

By B. H. Caudle, R. L. Slobod, E. R. Brownscombe

An earlier publication has discussed three methods lor obtaining relative permeability data on small core sample-: and the apparatus and technique for the capillary pressure displacement method. This paper describes the apparatus and technique for the solution gas and the dynamic displacement methods and presents a routine procedure for obtaining oil-gas and water-oil relative permeability data. Theoretical and experimental considerations are presented to show that the end effect commonly associated with the dynamic flow mechanism is extremely small where constant rates are employed in the flowing phase. An effect of flow rate on relative permeabilities obtained by the dynamic system is found only when gas is one of the flowing phases and this effect is ascribed to a form of channeling in the capillary system. The apparatus and procedure* used to obtain relative permeability data with three phases flowing are described and some preliminary results of the use of this method are shown. INTRODUCTION In a previous publication from this laboratory there appeared a brief discussion of the concepts behind three basic methods for obtaining relative permeability data.' These three methods were called the capillary pressure displacement method. the solution gas displacement method, and the dy. namic displacement method — the names being suggestive of the type of process used for obtaining the desired saturation prior to making the permeability measurements. In the same publication, the apparatus and technique for the capillary pressure displacement method were described and some typical results obtained by this method were presented. This paper will present: 1. The routine procedure used to obtain complete relative permeabilitv data (In small core samples with two phasec flowing; 2. The experimental techniques for the solution gas and dynamic displacement methods for obtaining relative permeability data; 3. The results of some studies on the mechanism of fluid flow through consolidated porous media; and, 4. The preliminary results on the determination of relative permeability for a system in which three phases are flowing. TECHNIQUE AND APPARATUS FOR THE DETERMINATION OF RELATIVE PERMEABILITY WITH TWO PHASES FLOWING In order to obtain relative permeability data on a small core sample which will describe the various phases of reservoir depletion. it is necessary that the methods used duplicate, as closely as possible, the various mechanisms involved in rescbrvoir depletion. It is important that. in any type of relative permedbility determination. the core be originally at virgin reservoir conditions with respect to the fluids within the pore *paces. (for example. oil used to displace water from core until connate water saturation estahlished). and that the subsequent saturation changes in the core be analagous to tile reservoir depletion mechanism for which the data are to he used. PROCEDURE OF DETERMINING RELATIVE PERMEABILITY DATA WITH TWO PHASES FLOWING A standardized procedure has been set up for obtaining relative permeability data and other information on small core samples. This procedure essentially consists of 11 steps as shown below: 1. Determination of tile capillary pressure curve.'! This information is used to help select samples for relative permeability determinations and to charactrrize. in general. the pore size distribution of the sample. 2. Determination of the specific permeabilities to air, oil. and water. These values are those on which the relative pern~eahility calculations are based. 3. Reduction of the core to connate water by an oil drive using the high speed centrifuge. 1. Determination of the critical gas saturation value and the associated relative permeability to oil by the solution gas drive method. 5. Determination of the relative permeabilities to oil and gab in the region where both phases are flowing by the capillary presqure method. 6. Reduction of the sample to residual oil in the centrifuge by an air drive. and the determination of the relative permeability to gas at this point.

Jan 1, 1951

By R. L. Slobod, B. H. Caudle, E. R. Brownscombe

An earlier publication has discussed three methods lor obtaining relative permeability data on small core sample-: and the apparatus and technique for the capillary pressure displacement method. This paper describes the apparatus and technique for the solution gas and the dynamic displacement methods and presents a routine procedure for obtaining oil-gas and water-oil relative permeability data. Theoretical and experimental considerations are presented to show that the end effect commonly associated with the dynamic flow mechanism is extremely small where constant rates are employed in the flowing phase. An effect of flow rate on relative permeabilities obtained by the dynamic system is found only when gas is one of the flowing phases and this effect is ascribed to a form of channeling in the capillary system. The apparatus and procedure* used to obtain relative permeability data with three phases flowing are described and some preliminary results of the use of this method are shown. INTRODUCTION In a previous publication from this laboratory there appeared a brief discussion of the concepts behind three basic methods for obtaining relative permeability data.' These three methods were called the capillary pressure displacement method. the solution gas displacement method, and the dy. namic displacement method — the names being suggestive of the type of process used for obtaining the desired saturation prior to making the permeability measurements. In the same publication, the apparatus and technique for the capillary pressure displacement method were described and some typical results obtained by this method were presented. This paper will present: 1. The routine procedure used to obtain complete relative permeabilitv data (In small core samples with two phasec flowing; 2. The experimental techniques for the solution gas and dynamic displacement methods for obtaining relative permeability data; 3. The results of some studies on the mechanism of fluid flow through consolidated porous media; and, 4. The preliminary results on the determination of relative permeability for a system in which three phases are flowing. TECHNIQUE AND APPARATUS FOR THE DETERMINATION OF RELATIVE PERMEABILITY WITH TWO PHASES FLOWING In order to obtain relative permeability data on a small core sample which will describe the various phases of reservoir depletion. it is necessary that the methods used duplicate, as closely as possible, the various mechanisms involved in rescbrvoir depletion. It is important that. in any type of relative permedbility determination. the core be originally at virgin reservoir conditions with respect to the fluids within the pore *paces. (for example. oil used to displace water from core until connate water saturation estahlished). and that the subsequent saturation changes in the core be analagous to tile reservoir depletion mechanism for which the data are to he used. PROCEDURE OF DETERMINING RELATIVE PERMEABILITY DATA WITH TWO PHASES FLOWING A standardized procedure has been set up for obtaining relative permeability data and other information on small core samples. This procedure essentially consists of 11 steps as shown below: 1. Determination of tile capillary pressure curve.'! This information is used to help select samples for relative permeability determinations and to charactrrize. in general. the pore size distribution of the sample. 2. Determination of the specific permeabilities to air, oil. and water. These values are those on which the relative pern~eahility calculations are based. 3. Reduction of the core to connate water by an oil drive using the high speed centrifuge. 1. Determination of the critical gas saturation value and the associated relative permeability to oil by the solution gas drive method. 5. Determination of the relative permeabilities to oil and gab in the region where both phases are flowing by the capillary presqure method. 6. Reduction of the sample to residual oil in the centrifuge by an air drive. and the determination of the relative permeability to gas at this point.

Jan 1, 1951

By R. F. Steigerwald

The effects of heat transfer on the corrosion behavior of type 304 stainless steel in boiling water have been studied. Heat transfer conditions increase the tendencies of the stainless steel toward stress-corrosion mucking when the water is contaminated with Cl-. Surface preparation is the most important variable in determining the severity of the stress-corrosion problem in water with a given Cl- content. Heat treatment, chemical cleaning, and degree of wet film boiling also affect the corrosion of stainless steels used as heat transfer surfaces in boiling water. An up-paratus for corrosion testing under controlled heat transfer conditions is described. THE principal objective of this investigation was to study the corrosion behavior of AISI Type 304 stainless steel in boiling high-purity water under conditions of heat transfer. The principal variables in the study were: a) boiling conditions: limited boil, agitated boil; b) metallurgical structure: annealed or sensitized; c) surface condition: rolled, pickled, or ground. The results of the study should elucidate the role of heat transfer in the corrosion of stainless steel in boiling high-purity water and provide a base line from which to assess the severity of this type of corrosion. Although there has been an investigation of the effect of heat transfer on the corrosion behavior of stainless steels in alkaline waters,' work on the corrosion of stainless steels under heat transfer has been largely confined to various acid solutions.'-4 Furthermore, the study of the corrosion of stainless steels in high-purity water has been generally restricted to auto-clave and instream testing in superheated (e.g., 300°C) water and steam.5'6 Cooling water problems led to this study of the corrosion behavior of type 304 stainless steel in high-purity water at its atmospheric boiling point. In addition to the effects of heat transfer, this study also considered the influences of the type of boiling,7 metallurgical structure, and surface condition on the corrosion behavior of stainless steel in high-purity water. Two boiling conditions were investigated in this study: a) limiting boiling, i.e., when the heat-transfer surface had just reached the boiling point and boiling nucleated randomly over the specimen surface and b) agitated boiling, i.e., when a mild degree of superheat had been achieved on the specimen surface and boiling occurred generally over the specimen surface. Both boiling conditions are broadly classified as wet-film boiling. Originally, this program included the study of a third type of boiling, dry-film conditions. At dry-film boiling the temperature of the heat transfer surface is high enough so that it is covered with a continuous film of steam. Experimental difficulties made it impossible to study this kind of boiling with the available apparatus. Since surface condition affects heat transfer rates, three typical surfaces were chosen for study: a) as-rolled, the 2B finish received from the supplier, b) as-pickled, 30 min in 8 pct HNO3-1 pct HF, and c) as-ground on 120 grit paper. In order to evaluate the effect of improper heat treatment or welding on hot wall corrosion, both annealed and sensitized mi-crostructure were included in this study. EXPERIMENTAL Test Apparatus. The particular problems of interest in this investigation required a knowledge of the thermal gradient through the test specimen. From this gradient, the heat flux to the surface and the surface temperature could be determined. In order to satisfy this need, an apparatus similar to the boiling-disk apparatus of Fisher and whitney2 was designed. The solution is contained in a thermally-insulated, steel pipe lined with TEFLON resin. A stainless steel _______;________________________________________

Jan 1, 1970

By P. F. Allen

WITH capacity of 51,000 tpd, the Morenci concentrator produces approximately 49,000 tons of tailing for final deposition. Disposal involves distribution of thickened tailing to dams in such a manner that solids can be used for dam construction and water can be impounded for reclamation. During early operation, although tonnage treated was lower, it was necessary to use orthodox disposal practices in the areas available for tailing. Trestles mounted on a series of dams, constructed of borrow material, carried the pipelines from which tailing were spigoted behind the dams. When adequate disposal areas were finally established, it became desirable to look for more efficient methods. The idea of placing the distribution pipe or manifold directly on the crest of the dam was advanced in 1945. After a period of testing, that procedure in modified form replaced the older trestle arrangement. Marked economies resulted, and time required to prepare dams for succeeding storage cycles was greatly reduced. The tailing disposal area for the Morenci concentrator lies south and southwest of the concentrator building. Ample storage space is available. A wide valley contains three sharply defined ravines lying on an average slope of 4 pct. The more central of these ravines, and the largest of the three, is known as Morenci canyon, which provides substantially more tailing storage area than the other two. Stargo canyon lies to the west; the other is appropriately named East canyon. Total area of the tailing disposal site is nearly 31/4 sq miles, or about 2000 acres. The storage area in use was somewhat more than 850 acres at the end of 1954, or 16 acres per 1000 tons of tailing to be stored daily. At the present time none of the east side dams are in regular use but they are available in emergency. There are five dams on the west side (in Morenci and Stargo canyons) as well as two auxiliary dams adjacent to No. 4 West and No. 5 West. This has made it possible to concentrate men and equipment in a smaller area with consequent savings in both manpower and machinery. Tailing Thickening: Tailing from the flotation process reaches the thickeners with a solid content of about 18 pct. The launder carrying this pulp is subdivided at a central point into seven launders carrying a proportional share to each of seven tailing thickeners, which are located in Morenci canyon close to the concentrator. Five of these thickeners are 300 ft diam and two are 325 ft diam. Thickeners are of the peripheral traction type and rakes travel at the rate of one revolution in 37 to 39 min. The entire installation provides 500,000 sq ft of settling area, or approximately 101/2 sq ft per ton of tailing to be thickened daily.

Jan 1, 1957

By Chester O. Ensign

Many publications to date have advocated under- seas mining operations, optimistically overlooking the paucity of information on mineral distribution and the ocean environments in which minerals occur. Such articles (smattered with opinion, as is this article) are herein tempered by my more conservative views on the economics of mining under the seas. For purposes of this paper, underseas mining refers only to the deeper surficial deposits of the continental shelf and the deep sea floor, i.e., the deposits of phosphorite and manganese nodules.

Jan 9, 1966

By Harry M. Mikami, A. Gene Sidler

Chemistry of the evolution of materials in contact with copper converter tuyeres is delineated by means of analyses of periodic punch rod samples taken during a converter cycle. Lining samples from known peripheral and end locations from three converters were investigated chemically and petrographically. One set of eight specimens representative of all lining parts was removed for study before completion of the campaign. Purely surface removal by slag action is minor. Slag filling of interconnecting cracks extending to the hot face results in a "stoping'' action which shapes the hot face contour and is a significant factor. Major wear mechanism is believed to be copper metal slabbbing caused by metal first penetrating joins and invading fractures or impregnating brick structure laterally from the joints. Importance of lining design and joint fit are emphasized. New laboratory tests are indicated. In the copper converter, molten matte, which is essentially a solution of iron and copper sulfides, is blown with air to produce blister copper. During the first stage of the process the FeS component is oxidized to SOz and FeO, the latter combining with a siliceous flux to form a predominantly ferrous silicate slag. Successive increments of matte and flux are charged, blown, and skimmed of slag until sufficient CuzS ("white metal") has accumulated. This white metal is then blown to copper metal in the final or blister-forming stage by the oxidation of sulfur to SOz and the reduction of combined copper to metal. The reactions of both stages are exothermic so provide the required heat. Temperature is controlled by cold scrap copper, flue dusts, smelter reverts, and so forth. Considerable vari- ation in practices occur depending on the type of converter, grades of the matte and flu, and other factors. Lathe and Hodnett's' survey of world converter practices gives much information on these variations and their effects on the refractories. Principles of converting chemistry are presented by Newton and wilson,' Ruddle,' and schuhmann. Most copper converting occurs within the temperature range 2100" to 2370°F although individual smelters report1 ranges from as low as 1700" to 2240°F to a high of 2200" to 2400°F. Temperature intervals reported from beginning to end of blow varied from 45" to 540°F. Average temperature range was 2030" to 2260°F and the average interval 250°F During the matte-blowing stage varying amounts of magnetite (FeO.Fe,O,) are formed in the slag as suspended crystals and also the liquid portion of the slag will contain, in addition to ferrous silicate, some Fe20s which adds to the potential magnetite formation if the temperature falls. This is a component of the so-called "dissolved magnetite" often referred to in the literature. Although the slag may contain minor amounts of CaO, A1209, MgO, and alkalies, the principal components are Fe0-Fez03-SiO,. The phase equilibria relationships of this system have been elucidated by Muan~ and Schuhmann, et a1.' These data and estimates of converting atmospheres by schuhmann4 are useful tools in studying slag behavior. It would appear that in many cases reported magnetite contents of slags are apparently higher than actually is present at operating temperature. This is probably because much of it is formed during slag solidification. The quaternary systems which have Mg-0,1,0,' and addition to iron oxides and silica are also of interest in considering the reactions of the slags with basic refractories. The formation of magnetite has an important interrelationship throughout the pyrometallurgy of copper (Mossman,' Gronningsater and Drummond," Ruddle,' Elwood and Henderson") but its presence in the converter particularly relates to operating efficiency and lining life in certain instances. Archi-

Jan 1, 1963

By B. E. Terkelsen, B. J. Piearcey

A study has been made of the effect of unidirectional solidification on the creep behavior, stress-rupture properties, and thermal shock resistance of four nickel-base superalloys. The alloys Mar-MZOO, B-1900, IN 100, and TRW 1900 show improved rupture ductility and thermal shock resistance when tested with the columnar grains parallel to the major stress axis during test. The relative improvement in creep-rupture properties depends on the intrinsic strength of the alloy, a property which depends on composition, heat-treatnient, and crystallographic orientation. The data clarifies some of the factors affecting the properlies of the cast nickel-base superalloy. COMPONENTS designed for high-temperature use have, in recent years, been fabricated by precision casting techniques using nickel-base alloys developed specifically for use in the conventionally cast condition. This development was a result of both the increasing complexity of the component and the recognition that high-temperature strength was incompatible with workability. The use of castings can be economically favorable, but, more important, the recent complex designs of air-cooled gas turbine blades and vanes in alloys which possess the necessary high-temperature strength cannot be forged. Common modes of failure of high-temperature components are excessive creep, creep rupture, and thermal fatigue. If rupture occurs then the mechanism is usually by inter crystalline cracking along those grain boundaries oriented transverse to the major stress axis. In the stronger alloys, rapid propagation of intercrystalline cracks result in apparent premature failure demonstrated by the absence of third stage creep in a creep-rupture test and low rupture ductility. Tensile ductility shows a similar trend, that is, decreasing ductility with increase in strength. It is not surprising, therefore, that increases in creep strength have only been obtained with a loss in resistance to thermal shock, a property which shows a dependence on tensile ductility. VerSnyder and ~uard' showed that the application of unidirectional solidification to a brittle Ni-Cr-A1 alloy both improved the rupture life of the alloy and increased rupture ductility. Since this casting method results in columnar grains, it appeared that the solution to the lack of ductility in nickel-base alloy components was the elimination of the source of failure, namely the transverse grain boundaries. This concept was recently developed2 to produce cast-to-size gas-turbine blades and vanes consisting entirely of columnar grains oriented parallel to the major stress axis of the component. Not only did the process impart increased rupture life and ductility to the components, but it also increased their resistance to thermal shock. During this development, the effect of unidirectional solidification on the properties of several alloys was investigated. The resulting data allows certain conclusions to be drawn regarding the factors affecting the creep and stress-rupture properties of the cast nickel-base superalloy and also its resistance to thermal shock. Detailed information was obtained on the alloys Mar-MZOO, B-1900, In 100, and TRW 1900. The composition of the alloys studied are shown in Table I. MATERIAL PREPARATION AND TESTING The conventionally cast alloys are cast as +-in.-diam bars in innoculated shell molds under conditions designed to maintain control of grain size. Unidirec-tionally solidified casting were produced in the form of 3-in.-diam ingots. Specimens from the latter were machined such that the axes of the columnar grains were parallel with the axis of the test bar, except in certain cases where the transverse properties of the material were being evaluated. The specimens were tested in an axial loading creep machine.' Temperatures were measured with thermocouples, attached just outside each end of the gage length, to assure uniform temperature along the entire specimen. Chromel/alumel thermocouples were used up to 1800"F and Pt/Pt-10 pct Rh thermocouples above 1800"F. The specimen temperature was recorded and maintained within i2"F throughout the test. Creep extensions were measured automatically with extenso-meters attached to ridges on the specimen and recorded continuously using linear variable differential transformers and multipoint recording equipment. MICROSTRUCTURE The microstructures of transverse sections of the four alloys studied are shown in Figs. 1 and 2. Fig. 1 shows optical micrographs of the alloys, both in the conventionally cast and unidirectionally solidified conditions. Each alloy displays a cored dendritic structure, a distribution of MC carbide, and the presence of the y — y' eutectic constituent.~ In the case of IN 100 and B-1900, Fig. 1 indicates that in these specimens the eutectic is degenerate. That is, it consists only of y' pools indicating that the y constituent has been solutioned during the cooling period after solidification. The major effect of unidirectional solidification on the microstructures of the alloys is a tendency to promote a more dendritic form of MC carbide and an increase in dendrite arm spacing, both effects being a result of the slower solidification rate in the unidirectional solidification technique. V, lec tron micrographs of transverse sections of the four alloys in the two cast conditions are shown in

Jan 1, 1968

By Larry Kaufman, Joan B. Berkowitz-Mattuck, Edward V. Claugherty

The oxidation characteristics of hafnium and zirconiunr diboride were measured between 1200 and 2200'K by a thermal- conductivity method which continuously ttzeasures the rate of reaction of oxygen with the diboride and by a metallographic air oridation method zuhich provides a measure of the total arr7ount of bovide conuerted to oxide for a given time interval. The oxidized specimens obtained from the tl~eritaal-coi~ductitrity method were also examined by quantitatire metal-lographic procedares. The significant results obtained in this investigation reveal that metal-rich compositions of lzafi~iutil diboride proride the most oxidation-resistatzt material up to 2000°K; hafnium diboride is tmre oxidation- resistant titan zirconium diboride at all tempevatures examined; the morphology of the oxide formed on H/B2 and Llie temperature coefficient qi. the oxidation rate constants change at the temperature of ttze monoclinic to tetragonal phase transition] in HfO2; the oxidation of neither HfB2 nor ZrB2, results iN catastrophic Jazlure at lorc. oxygen pressures; and pvefevetztial gvaLti boundary oxidation was not obsevued for either HfBi or ZYB, A comprehensive study of the high-temperature characteristics of refractory transition-metal di-borides is currently in progress. This program has included investigation of the physical, thermal, and thermodynamic properties of TiB2, ZrB2, HfB2, NbB2, and TaB2. In addition, aspects of the synthesis and fabrication of such materials have been studied. In view of the diverse nature of this research, a number of other laboratories have actively participated and contributed specific capabilities for analysis and characterization of these materials. As a consequence, an extensive description of the relevant properties of these compounds has emerged which is central in evaluating their high-temperature (1200" to 2500°K) performance. To date, information on thermodynamic stability, specific heat, and vaporization characteristics,1 hot hardness and electrical resistivity,1, 3 therma1 expansion:'4 and thermal conductivity 1, 5 has been presented. This information has been generated on materials of the highest purity (98.5 to 99.9 wt pct Me + B) and density currently available. Samples fabricated by zone melting6 and high-pressure hot pressing"3'7 techniques have been used to generate suitable specimens for all of the aforementioned studies. dation characteristics of the most oxidation-resistant of these materials, hafnium and zirconium diboride, is presented and a description of the synthesis and the experimental procedures used to prepare and characterize specimens is given. The high-temperature range under consideration (1200" to 2200°K) and the known dependence of oxidation characteristics on sample chemistry, density, and oxidation conditions required a close coupling of the synthesis, fabrication, and evaluation procedures.8 This was accomplished by continual surveillance of chemical composition of starting materials before and after specimen fabrication and by evaluation of density, phase constitution, and microstructural features prior to and after oxidation exposure. I) PROCUREMENT AND CHARACTERIZATION OF STARTING MATERIALS In view of the current state of the art in fabricating refractory boride materials, the methods used in preparing samples for the present study are given in detail as follows: starting materials were purchased in high-purity powder form and fabricated by high-pressure hot pressing into 0.40 by 1.00 in. bars from which oxidation specimens were obtained. The hafnium diboride used in this study was purchased from Wah Chang Corp.; the zirconium diboride from U.S. Borax and Chemical Co. These powders were routinely characterized by quantitative chemical analyses for metal, boron, carbon, oxygen, nitrogen, and iron, by qualitative emission-spectrographic analysis for trace impurities, by X-ray procedures for extraneous phase identification, and by powder densitometry for comparison with X-ray (theoretical) density. Hafnium and zirconium metal and elemental boron were also purchased as high-purity powders and characterized for impurities by emission-spectrographic analyses. The hafnium diboride was procured in three shipments which were designated as HfBl.g7(1), HfB1.88(2A), and HfB2.12(2). The indicated stoichiometry is based on the atomic ratio of total boron to total hafnium; the number in parentheses identifies the shipment number. Shipment 1 was 5 1b, shipment 2A, 1 1b, and shipment 2, 8 1b. The zirconium diboride was procured as a 20-1b shipment and designated as ZrB1.89(1). A small quantity of purified zirconium diboride was also supplied and designated ZrB1, 9(P). The averaged results for chemical analyses which were generally performed according to the procedures set forth in the compilation by KrieGe9 are presented in Table I. Qualitative spectrographic analyses indicated that Ca, Cr, Ti, Si, Zr (in H~B~), and A1 were present at levels between 0.01 and 0.10 wt pct. Other metallic elements were found to be less than 0.01 wt pct. Since it is virtually impossible to purchase these materials in the desired quantities (5 to 20 lb) as single-phase compounds it is necessary to obtain

Jan 1, 1968

By Charles R. Cavanaugh, John F. Elliott

The activity of nickel in liquid Pb-iVi alloys which are rich in lead was measured in the temperature region of 700° to 1100°C by means of the galvanic cell: The electrolyte used was stabilized zirconia. Tlze data were correlated using the a function, and a plot of the temperature coefficient aE/aT All subsequent calculations of the thermodynamic properties are based on these two functions. The activity, activity coefficient, and molar properties of mixing of nickel are reported. Nicke1 shows extreme positive deviations frorn ideality while lead shows a very slight positive deviation in the composition range studied The study of the activity of nickel in liquid Pb-Ni alloys reported herein was undertaken to explore the use of stabilized zirconia, an oxygen-ion electrolyte, with liquid-metal electrodes, and to obtain further information on the thermodynamic properties of the liquid binary Pb-Ni system. The cell The reversible electromotive force of the cell results from the difference in the chemical potential of the oxygen at the two electrodes: po, (left) - p~ (right) = -4E5 [I] The chemical potential of oxygen on the right is fixed by the activity of nickel in the solution and pure solid nickel oxide. That on the left is set by pure solid nickel in equilibrium with pure solid NiO. By definition: Since the chemical potential of nickel is related to the chemical potential of oxygen through the equilibrium constant for the formation of NiO from nickel and oxygen gas, the electromotive force of the cell is also expressed In this case, n is 2, E is the reversible potential of the cell, and 5 is Faraday's constant. The work of Kuikkola and wagnerl and Schmalz-reid2 has shown that the stabilized zirconia electrolyte is essentially an ionic conductor at the oxygen levels encountered in the experimental arrangement of the work, i .e., PG > 10-l7 atm. THE EXPERIMENTS The advantage of this type of reversible cell over those using a liquid electrolyte is the simplicity arising because the electrolyte also functions as one of the containing crucibles. A further simplification was the choice of the Ni (sat.)-NiO electrode as the standard. This permitted a ready check on the behavior of the electrolyte, as the potential of the cell must become zero when the right electrode becomes saturated with nickel, either because of a change of temperature or because of the addition of nickel to the electrode. It also permitted the potentials being measured to lie in the most satisfactory experimental range of 0 to 100 mv. Although it was not theoretically necessary, lead was included in the standard electrode as it assured good contact between the electrode and electrolyte. Cell Design. The general arrangement of the experimental cell assembly is shown in Fig. l(a) and the details of the cell itself are contained in Fig. l(b). The anode lead wire on the interior of the cell was connected to a coil of perforated sheet nickel. Within this coil were nickel oxide pellets which were held beneath the surface of the liquid Pb-Ni alloy. A disc of nickel oxide was held at the bottom of the external crucible (alumina) by means of the thermocouple protection tube. The nickel oxide disc and pellets were compressed dry at 10,000 psi and sintered at approximately 1000°C for an hour in air. A major experimental difficulty of reversible electromotive force cells with liquid electrodes is the selection of suitable materials for connecting

Jan 1, 1964

By J. E. Hove

The high temperature physical properties of graphite are reviewed and interpreted in the light of present day knowledge of the mechanisms affecting these properties. The thermal and mechanical behaviors only are discussed and, whenever possible, comparisons are made with other refractory materials. Possible further studies are indicated, including some carbide work. AS long as the term high temperature implied only temperatures up to about 1000°C, the materials problems which arose could usually be handled by fairly conventional metal alloy types, such as the Co-Cr-Ni superalloys, for which there exists a great deal of technology. Perhaps this temperature can still be considered an upper limit for normal applications, but it is certainly true that the number of abnormal applications is increasing rapidly. The advent, in recent years, of ram-jet and rocket missiles and of high power nuclear reactor heat sources has raised a host of questions concerning the basic problem of what material to use in the temperature range up to 2000°C and higher. While there are, of course, many metals, in the second and third transition series, which melt at considerably higher temperatures than this, these metals are, at present, pretty well excluded from practical use by other considerations, such as re-crystallization, chemical activity, or excessive plastic deformation. The behavior of metals, from the standpoint of dislocation theory, is just beginning to be understood and thus there is some hope for the future development of very high temperature metals, but the immediate problems would most logically appear to have solutions involving the nonmetals, such as the refractory ceramics and graphite. For this reason, there is presently a great deal of engineering and experimental research being performed on the latter materials, much of this research being exploratory in the sense of gathering new property data. The situation, so far as graphite is concerned, is somewhat more fortunate than with the other refractory solids in the sense that a great deal is already known about its basic properties. This stems both from the fact that the carbon-carbon bond has been of interest to chemists for a long time (and graphite can be considered as a very large aromatic molecule, if desired) and the fact that its properties, both as a function of temperature and of radiation damage, are of critical importance to nuclear reactor designers. It is still true, of course, that such fundamental questions as why graphite remains solid to such a high temperature and why it has such a high thermal conductivity cannot entirely be answered at the present time. It is, nonetheless, meaningful and instructive to consider such problems in the light of existing knowledge. This is what the present paper will attempt to do. Before going on, it may be appropriate to classify graphite and justify its discussion before readers primarily interested in metals. Graphite is comparatively unique among materials in that there is always a property or group of properties which precludes calling it either a metal, a semiconductor, or a ceramic. It has the high electrical and thermal conductivities of a metal, but the artificial, poly-crystalline types show a negative thermal coefficient of electrical resistivity, generally characteristic of semiconductors. On the other hand, semiconductors, by definition, show an ever increasing resistivity as the temperature is lowered, whereas graphite approaches a finite, and, indeed, a rather low resistivity in the region of 10°K and, furthermore, a good single crystal of graphite has a positive temperature coefficient, as for a metal.' On still another hand, its porosity and brittleness at lower temperatures would put graphite in the ceramic class although, unlike most ceramics, it is readily machinable and has a high resistance to thermal shock. All things considered, it is probably more nearly appropriate to call graphite a metal than anything else. Although certainly outstanding in some ways, graphite has its peculiarities and, especially if the reader is unfamiliar with the data, it is probably valuable to review some representative property variations at high temperature. This review is meant to be mainly illustrative and no attempt has been made to be exhaustive. Review of High Temperature Properties At ordinary pressures, graphite does not melt, but sublimes directly into the gaseous phase at about 3700°C. Although the phase equilibrium diagram is still in some doubt, graphite will melt, at a slightly higher temperature, at pressures in excess of about 100 atm. The chief difficulty of using graphite in an oxidizing atmosphere is that the reaction rate becomes quite high at fairly low temperatures. If a threshold oxidation temperature2 is defined as the temperature at which graphite loses 1 pet of its weight in 24 hr, the value in air is 450°, the value in steam is 700°, and the value in carbon dioxide is 900°C. Efforts are presently being made to raise this threshold temperature either by impregnation with a retardant of some type (sodium tung-state and phosphoric acid, for example) or by a suitable metal or oxide coating. It is probably fair to say that, to date, these attempts have not shown any outstanding success in all respects. Most commercial graphites are fabricated by impregnating a carbon flour (say of coke or lampblack particles) with some type of hydrocarbon

Jan 1, 1959

By T. Gleason

Problems involved in applying wet scrubbers to gas cleaning coal dust from thermal dryers are reviewed. Careful consideration of all the elements going into a modem coal preparation plant is required in view of the increasing difficulty of applying suitable gas cleaning equipment. This problem arises not only from the presence of finer coals to be handled, but also from the pressures applied by both the general population and the plant operators to improve the standard of gas cleaning performance. The Peabody scrubber is presented by the author as a machine designed to help improve this cleaning operation. Wet scrubbing of fine coal from thermal dryers poses a number of problems in adapting the gas cleaning equipment to the fine particulate matter. Among them are: 1) Dust in gases leaving the thermal dryer cyclones is often extremely fine with high percentages of total dust loading less than 1p in size. 2) Flue gas entering the scrubber is corrosive since the coal fired in the thermal dryer furnace is in the range of 0.7% by weight sulfur or higher. Therefore, comparatively high cost stainless steel alloys or corrosion resistant linings are required for a satisfactory service life. 3) Requirements for residual coal loadings leaving the gas scrubber are continually being lowered, while modern coal preparation operation is imposing heavier burdens on the collection system through introduction into the thermal dryer system of very fine coal previously not recovered. The advent of flotation systems in increasing numbers is typical of this trend. 4) Installation of a scrubbing system on thermal dryers is made primarily to reduce air pollution and product recovery value is of little or no value. Therefore, the operating costs of gas pressure drop and water requirements must be held to a minimum. We have, then, the basic situation which calls for comparatively high cost stainless steel alloy wet scrubbers, which must be highly effective in removing coal fines particularly in the 0 to 5-p size range. Further, the standards of scrubber performance are continually being raised towards the level where gas discharged from the scrubbers must be essentially free of any coloration due to residual dust. In view of the highly refractive nature of fine coal dust, residual loadings of 0.01 grains per cu ft or less are required to provide a color free discharge gas. In the present specifications under consideration a residual coal loading of 0.05 grains per cu ft would be considered color free, since the discharge gases are saturated in the range of 150°F. The steam plume acts as a masking agent at the point of discharge, and upon dissipation of the 150° saturated vapor stream, the effluent gas stream could be essentially color free. The specification under consideration calls for residual solids loading of 0.05 or less grains per cu ft, given a coal size distribution shown in the basic data in Table I. It is noted that the dust laden coal stream has a size distribution by weight of 33% in the 2 to 5-p size range and 55% in the 0 to 2-p size range. The particle size distribution given in the specifications does not detail the percent by weight less than 1-p in size, and more important, the size distri-

Jan 1, 1963

By J. B. Fletcher

The Miami mine first started operations in 1910. For convenience, the history of the orebody can be divided into the following categories (Fig. 1): 1) 1910 to 1925: 24.4 million tons of high grade ore, mined by top slicing, sublevel caving, etc. 2) 1926 to 1954: 102 million tons of low grade ore, mined by block caving.

Jan 1, 1961

By W. A. Clark, E. H. Dresser

ORE from the Minnesota iron ranges is transported from the mines to the loading docks on Lake Superior over four different railways: the Great Northern, Northern Pacific, Soo Line, and Duluth, Missabe and Iron Range, with hauls varying from 60 to 110 miles. For this service a large amount of specialized equipment is used. The steel ore cars are of the hopper type, 24 ft. long, to dump into alternate pockets of the docks, these pockets being 12 ft. long to correspond with the 12 or 24-ft. spacing of the boat hatches. The more recently con-

Jan 1, 1941

By Paul Soros

The cost of shipping British coal by water to domestic and ex- port users has been expensive. The traditional transportation system functioned as follows: coal in up to 50 different grades was accumulated in railway cars at several loading ports; on the arrival of a vessel, cars were dumped in the desired order to produce the required blend. It was a direct rail- road-to-water interface. Railroad freight was high because of the poor utilization of the large number of small (14, 18 or maximum 28-ton capacity) hopper cars required. Ocean freight was high because the ships were small, mostly on the order of 1500-3000 dwt and even these took a long time to load. Assembling and loading larger cargo presented a challenge in logistics to the ports, the railways and the coal washeries. The accommodation of larger bulk carriers was hampered by a tidal range of up to 24 ft which led to the development of impounded harbors, with locks that limit the size of vessels.

Jan 12, 1973

By F. S. Jr. Norcross

MANGANESE has long been considered one of the United States' most important strategic raw materials. Its indispensabil-ity in steel manufacture makes it vital to the nation's industrial life. Coupled with this indispensability is the fact that domes-tic producers have not been able as yet to supply more than a small part of the nation's manganese needs; consequently the United States has had to depend upon such distant foreign sources as the U.S.S.R., British India, the African Gold Coast and Brazil for the major portion of its ore. The great bulk of the mineral is con-sumed in the form of ferromanganese, an alloy that averages 8o per cent manganese and 20 per cent mainly iron and carbon. Manganese is used as a deoxidizer and desulphurizer in steel manufacture. By combination with the residual oxygen and sulphur of the bath, it helps to produce a clean, sound metal. Approximately 14 lb. of manganese, it is estimated, is used in making one ton of steel. For standard-grade ferromanganese, the ore should have a minimum of about 48 per cent Mn and preferably more. Beneficiation methods have not yet been developed for making the immense low-grade deposits in the United States salable at prevail-ing prices.

Jan 1, 1940