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Jan 1, 1953

By Leo F. Reinartz

Part II of a four-part series on the history of steelmaking in the US, points out the inadequate safety and living conditions that existed in steel mills at the turn of the Century. Also defined are furnace and process developments. OPERATIONS in steel plants today are highly mechanized. Men work in light, clean, orderly melting shops, making it difficult for old timers to convince young men that primitive, hazardous conditions existed in steel plants at the turn of the century. Working conditions then were very poor as compared to present day standards. In small plants especially, sanitary, locker, and washroom facilities, first-aid practices and stations were un- known Accidents were frequent and severe. Workers had a fatalistic attitude toward getting hurt. He who had an accident was looked upon as a hero. A dirty bandanna often served as a bandage. Infections were frequent. Electric cranes were in their infancy and broke down often Cables had not as yet replaced chains. Pig iron and scrap iron were loaded by hand in the stockyard, and stockyard locomotives were un- known; mules served as the usual motive power. It was not unusual to see recorded a delay of ½ hr in charging a furnace because of a balky mule. Furnace operations A few plants had primitive charging machines, but most furnaces were charged by placing scrap or pig iron on the paddle of a long peel, which rested on a bar across the furnace door opening. Laborers at the handle end of the peel, using the bar as a fulcrum, would heave the material into the furnace by a down and sideward motion of the peel handle. In time they became expert in placing these materials in the furnace, but it was hard, hot work, and a long time was required for charging. Cold charges of 25 tons required more than 12 hr for melting and re- fining the steel. Ports, doors, and frames were not water cooled. The charging and working area in front of the furnace was covered with steel plates. They were hot and often warped by the intense heat of the un- insulated checker chambers directly below. In the summer, working conditions on the charging floor were almost unbearable. Silica refractories were of poor quality. Because of this, and the inadequate training of furnace men in fuel control and furnace operations, roofs, front and back walls, and ends burned out rapidly. Dolomite machines were unknown; consequently, furnace banks and hearths were fettled with dolomite by the use of hand shovels. The round system required six or more men. Each man took a shovelful of dolomite and, in his turn, deposited it on the back wall and bank by a dexterous forward swing and twist of the shovel. The upward swing of the shovel partially protected his face from the searing heat of the furnace coming out through the wide-open door. Considerable skill and stamina were required to do this job properly. Reverse valves, usually of the cast-iron butterfly type, were located below the charging floor. They were operated by long levers on the charging floor level men they became warped, because of heat and abuse, great strength and skill were required to reverse them. Furnace operations were difficult. The quality and quantity of producer gas coming from irregularly stoked, hand-operated gas producers was uncertain and unreliable. Furnace Linings and ports were quickly burned out. Poor bottom and side-wall refractories, indifferent and inexperienced crews, as well as irregular re-

Jan 1, 1961

By E. F. Bradley, R. I. Jaffee, H. R. Ogden, E. S. Bartlett, D. N. Williams

The mechanical properties of solid-solution-strengthened columbium alloys have been assessed as a function of alloying additions. Studies included the effects of tungsten, tantalum, molybdenum, and vanadium. Elevated temperature fabrication was required at alloying levels above about 15 pct W or 10 pct Mo. Tungsten, molybdenum, and vanadium additions increase tensile strength at room temperature and 2200°F, but tantalum additions exert little strengthening. Similarly, tungsten, molybdenum, and probably vanadium additions increase the ductile-to-brittle transition temperature, and tantalum additions decrease this parameter. The 2200°F stress-rupture strength is increased by tungsten and molybdenum additions; with 20 to 25 at. pct additions, 100-hr rupture strengths of 30,000 psi are obtainable. Small vanadium additions exhibit mild stress-rupture strengthening, and tantalum additions are innocuous. At 2500°F, tungsten additions retain stress-rutpure strengthening capability, but molybdenum additions are much less effective. Tantalum additions augment the stress-rupture strengthening of tungsten plus molybdenum additions at 2500°F. Of the refractory metals, columbium possesses specific potential for structural use in the temperature range from 2000" to about 2500°F. Desirable features of columbium are its good low-temperature ductility, ease of fabrication, oxidation mechanics (lack of a volatile oxide at moderate temperatures), good availability and reserves, and relatively low density. However, alloying is required to provide attractive strength at elevated temperatures. Published information concerning alloying be- havior of columbium relative to mechanical properties is sketchy, particularly in consideration for long-time applications at temperatures in excess of 2000°F. Only a few stress-rupture data at temperatures from 2000" to 2500°F have been reported;'-' these are too meager to allow rationalization of the effects of various alloying additions on creep or stress-rupture properties. Additional published data do, however, give some insight toward understanding of systematic alloying behavior for columbium relative to low-temperature strength4-' and ductility,' and elevated temperature tensile behavior.4,6 This paper is intended to augment previous knowledge, and to promote understanding of the alloying behavior of columbium for long-time structural service at elevated temperature. BASIC CONSIDERATIONS Solid-solution strengthening is recognized to be of prime importance in improving strength in columbium-base alloys. Other strengthening mechanisms may be (and are, in current alloys) used to augment solid-solution strengthening. As strengthening results primarily from lattice distortion, the strengthening effectiveness per atom depends upon atomic size mismatch between solvent and solute. Another factor in this regard is conformance to ideal solution behavior in the solid solution. Thus, for example, despite appreciable differences in the degree of mismatch between tungsten (5 pct), molybdenum (5 1/2 pct), and vanadium (7 1/2 pct) in solution in columbium, all are about equally effective in straining the columbium lattice at room temperature.'-' Similarly, tantalum additions do not strain the columbium lattice, and little strengthening is expected. Size effects being equal, maximum solution strengthening at high temperatures is anticipated to result from the addition of elements that increase the melting temperature of columbium. This expectation is based on an increase in the electronic bonding forces exhibited in the transition metal series as electronic structures approach those of the Group Vl metals. Of the metals that exhibit ex-

Jan 1, 1963

By Barry H. G. Brady

A state of stable equilibrium is required in a mine structure to ensure that small increases in the mined void are accompanied by only small displacements of the rock mass. Methods of determining the stability of equilibrium in a rock mass currently require a geometrically regular stoping layout, and introduce a number of simplifying assumptions. The method reported in this paper models the mine near-field using Finite Elements, and the far-field using Boundary Elements. The stability of equilibrium in the modelled structure can be assessed directly from the value of selected principal minors of the global stiffness matrix.

Jan 1, 1981

By Orson Shepard

THE term "electrocapillary amalgamation" is used in this paper to designate amalgamation processes that depend upon electrocapillary phenomenon; i.e., the action of an electric current upon the surface tension of mercury at the contact with aqueous solutions. Electro-capillary amalgamation is selected as a name for these processes because the electrocapillary phenomenon has been found to be the effective agent in the use of sodium amalgam, as well as in the various processes using an electric current from a source outside of the amalgam. Amalgamation processes that depend upon supplying an electric current to the amalgam from an outside source, such as batteries and generators, have previously been called electrical amalgamation processes. There has been a tremendous amount of experimental work done on amalgamation processes involving the use of an electric current, as shown by the large number of patents issued on these processes: the earliest in 1885 and the latest in 19341. Regardless of all the experimental work, the fundamental principles causing the operation of electrocapillary amalgamation processes have not been described. The explanation usually given is that an electric current keeps the amalgam bright and clean. Patent No. 328532 states: It is well known that when amalgam plates are used for collecting gold and silver from their ores the surfaces of these plates are liable to become tarnished or sickened by certain substances contained in the ores or in the current of water which is employed to carry the ore over the plates, and that in this condition they are unfitted for amalgamating the particles of gold and silver. To prevent this and to keep the surfaces of the amalgamation plates always bright and in a better condition for catching and amalgamating the particles of gold and silver I employ electricity in the following manner:. . . A similar explanation is given 49 years later, in patent No. 1953364: The sodium (Na) ions lose their charge at the cathode becoming sodium atoms, which do not react with the electrolyte, but follow the grounded electrical current through the mercury body producing in their passage sodium amalgam and liberate themselves in the amalgamation compartment when brought in contact with the fed

Jan 1, 1936

By L. W. McKeehan

The occurrence of twins in large ferrite crystals, made by a new process, was reported in a recent note.' This paper describes a typical case of such twinning and suggests, on the basis of the observed facts, why smooth slip-planes are rarely observed in this metal. Method of Preparation The material in which the crystals here dealt with were grown was made from 1/8in. Armco iron welding rod containing C, 0.04; S, 0.037; P, 0.003; Si, 0.008, and Mn, 0.02 per cent. This rod was cold drawn into wire about 1 mm. dia. A piece of this wire was supported vertically and was locally heated in hydrogen at atmospheric pressure to about 1400" C. by an alternating current (60 cycles per sec.) of about 35 amp., passed through it between a pair of traveling contacts about 8 cm. apart. The rate of travel for the case in hand was 12 cm. per hr. After some 30 cm. of the length of the wire had been heated and cooled in this manner the whole wire was immersed for a few seconds in dilute nitric acid, not restrained by alcohol. Etching was continued until, as nearly as could be judged by eye, the original smooth cylindrical surface of the wire was no longer capable of specular reflection. Measurements The wire in the etched state was next mounted in a goniometer of special form which allowed the measurement of the spherical coordinates of the normals to any plane surfaces left by the etching. These coordinates were most conveniently a polar distance, 8, from one direction of the wire axis, and an azimuth or longitude, ?, from an arbitrary prime meridian. The region to be described more particularly is shown at a low magnification in Fig. 1, which gives two different views, differently illuminated to show the spatial relationship of a crystal occupying most of the part shown and of an inclusion, or rather a series of three inclusions suspected of being twins based on the principal crystal.

NEW YORK LOCAL SECTION Executive Committee L. W. FRANCIS, Chairman WILLARD S. MORSE, Vice-Chairman THOMAS T. READ, Secretary, Woolworth Bldg., New York, N. Y J P. A. MOSMAN, Treasurer Louis D. HUNTOON Since the annual meeting in February, the New York Section of the Institute has held three meetings. The meeting-on March 10 was held in conjunction with the American Society of Mechanical-Engineers and the American Electrochemical Society, at the Engineering Societies Building. The papers of the evening were devoted to records of progress in the Processes for the Photographic Reproduction of Natural Colors. The speakers of the evening were F. E. Ives, one of the earlier workers in color photography, Westley Allison, C. W. Robinson, George F. Clyfton, John B. Taylor, and Henry Hess. The April meeting was held on April 22 at the Institute headquarters, and the topic for discussion was Sanitation in Mining and Metallurgical Work. The principal paper was by J. W.. Luther, chief surgeon of the New Jersey Zinc Co. This was followed by a similar paper by Charles L. Close, secretary of the Welfare and Sanitation Committee of the United States Steel Corporation, and by an account of the sanitation work done in Cuba by the Spanish-American Iron Co., which was read by the Chairman, in the absence of Charles F. Rand. Following these papers general discussion was indulged in.

Jan 6, 1914

CONTENTS PAGE ANDERSON, ROBERT J., and ENOS, GEORGE M.-Corrosion of Brass as Affected by Grain Size. Discussed by Henry S. Rawdon, Robert J. Anderson, Francis B. Coyle, William B. Price, and W. R. Webster 1 RAWDON, HENRYS., and MUTCHLER, WILLARD H.-Effect of Severe Cold Working on Scratch and Brinell Hardness. Discussed by W. H. Bassett, John Livermore Christie, John R. Freeman, Jr., W. R. Webster, William B. Price, Norman B. Pilling, D. J. McAdam, Jr., F. G. Smith, Zay Jeffries, F. E. Carter 3 WILLIAMS, ROBERT S., and HOMERBERG, VICTOR 0.-Relation of Heat Treatment to the Microstructure of 60-40 Brass. Discussed by 0. W. Ellis 14 Corrosion of Brass as Affected by Grain Size Discussion of the paper of ROBERT J. ANDERSON and GEORGE M. ENOS, presented at the New York Meeting, February, 1924, and issued as Paper No. 1282, with MINING AND METALLURGY, December, 1923. HENRY S. RAWDON,* Washington, D. C. (written discussion).-So numerous and so varied are the factors that affect the corrosion of metals that particular care is necessary in corrosion tests to eliminate so far as possible all extraneous factors. It appears to the writer that the question may well be asked as to whether all the necessary precautions have been observed in this investigation. It may be that the points to be mentioned were considered by the authors and found to be insignificant; however, there is nothing in the report to show this.

Jan 5, 1924

By S. W. MILLE

GEORGE F. COMSTOCK,* Niagara Falls, N. Y. (written discussion?).¬I have recently had the pleasure of reading Mr. Miller's interesting paper, and would like to call attention to a reference to this subject which apparently has escaped his notice. It is an abstract of a German research on the subject of nitrogen in steel, and appeared in the Iron Age of Feb. 17, 1916, page 432. Photomicrographs of needles such as Mr. Miller found in his welds are given, and their identity is discussed. The conclusion reached is that the needles are slip lines due to the brittleness of the ferrite crystals caused by their absorption of nitrogen. The deformation necessary to develop the slips is supposed to be accomplished either in cutting or polishing the microsections or by cooling strains after welding. It seems very reasonable to expect that nitrogen would he absorbed by steel in either electric or oxy-acetylene welding, and the reference I have mentioned gives instances of many unusual structures resulting from the presence of considerable nitrogen with carbon in steel. But the nitrogen is .rapidly given off from steel by ordinary annealing in air, hydrogen or vacuum, and this would explain the disappearance of Mr. Miller's needles after annealing. I think the conclusion that the needles are cementite might well be revised in view of this German work on nitrogen.

Jan 5, 1918

By Albert W. Giles

The splitting of the coal by partings is a familiar feature of many coal beds. The partings are normally argillaceous, more rarely sandy or calcareous. The material is usually fine-grained, less frequently coarse-grained to conglomeratic. Many partings are wedge-shaped, others are lenticular, and in some coal beds thin partings but one or two inches thick persist as thin sheets throughout areas of regional extent. The origin of the partings differs, and in some cases is obscure and uncertain. Origin of Thick Partings Wedge-shaped Partings Wedge-shaped partings are normally of indefinite linear extent but of short transverse section. They are developed adjacent to the borders of the original peat-forming swamp or around islands formed within the swamp, hence their presence is indicative of the approximate limit of the coal bed or of an interruption in the continuity of the coal bed. Following deposition of the parting gradual reestablishment of swamp conditions is followed by burial of the parting with accumulating peat. Partings developed adjacent to the borders of swamps normally thicken toward the periphery of the swamp and represent either detrital materials carried in from adjacent land areas during floods or materials carried in by advancing waves and currents after a barrier confining the swamp had been breached by the waves. Partings formed in the manner first mentioned should become coarser and more arenaceous toward the source of supply of the detrital materials, and the overlying and underlying coal should gradually grade into carbonaceous shale as the margin of the original swamp is approached. Partings formed by advance of waves across a barrier should be largely or entirely arenaceous, thin wedges of short longitudinal section, possibly with fossils of marine or brackish affinity. The subjacent coal normally should "pinch out" against the barrier, and the overlying coal continue to the barrier, or even extend across it, depending on the geographic conditions established following the breaching of the original barrier. Islands may be formed in swamps in a number of ways. They may represent local uplift of the swamp floor during earthquakes, or

Jan 1, 1934

By John Furness Park

The mining district is located in the northeasterly part of Nevada, between the Jarbidge River on the west and the East Fork of the Jarbidge on the east. The northern boundary of the district is but a few miles south of the Idaho state line—the gold-bearing area extending from this point south, for 5 or 6 miles. • The Jarbidge Mountains, in which the ore deposits occur, range from 5000 to 11,000 ft. in elevation, the most important mines being situated about 7000 ft. or higher. The town of Jarbidge lies along the Jarbidge River and is reached by stage from Rogerson, Ida., the nearest railroad point. During the summer months, the camp may be entered from the south by way of Deeth, Nev., but no regular transportation facilities are available over this route. History The mineral deposits were not discovered until 1909, when D. A. Bourne, panning along the river bank, found gold in. the gravel at the mouth of a small stream flowing into the Jarbidge. He prospected in the vicinity of this stream, later known as Bourne Gulch, and shortly after located the North Star claims. During the following spring and summer (1910), the camp of Jarbidge grew from nothing to a town of 2000 people and the hills surrounding it were practically all taken up by mining claims. Most of the work done during the first year or two consisted of trenching and open-cut prospecting. Tunneling was started on a number of claims and many veins were uncovered. Mills were built and operated on a few properties, notably the Pavlak and the North Star. These ran only a few months, however, when they were closed down because of extraction and financial difficulties. A period of development followed in which the majority of the present producing mines were opened. The Elkoro Mines Co. acquired a number of claims in 1915 and started work on the present mill in 1917. Since that time other properties have been taken over until this company is by far the largest operator in the district. Only one other company is now actively engaged in mining, the Bluster Mining & Milling Co., which has

Jan 1, 1925

By D. R. Mash

A strong yield point with attendant enhanced mechanical properties was found in commercially pure beryllium under certain conditions of heat treatment. Beryllium specimens also responded to both quench and strain aging treatments. Based on these results, a possible means of obtaining increased normal temperature mechanical properties is suggested. COMMERCIALLY pure beryllium has been found to exhibit the yield point phenomenon and several other aging manifestations under certain conditions of heat treatment. This behavior is not surprising in view of the present accumulation of experience regarding such effects in numerous metals; but in addition to extending this experience to include beryllium, the present study is of interest because aging effects are generally associated with the presence of small amounts of solute elements. The well known lack of tensile ductility in beryllium at normal temperatures is also considered to be due to impurities in some way. In the present investigation, the view was taken that beryllium of commercial purity (greater than 98 pct) should be considered as a dilute alloy and that precipitation phenomena may well exist which could lead to enhanced mechanical properties. In connection with this possibility, published data on the variation of mechanical properties with temperature are of interest. For example, Fig. 1 illustrates the variation of ductility (percentage of elongation) and ultimate strength as a function of temperature for beryllium of various histories.* Although these curves are somewhat schematic in nature, they clearly indicate the possibility that precipitation of an unstable phase and/or aging effects occur during tests in the region 400" to 700°C. The existence of such behavior should be recognized as affecting the properties of the commercial material and perhaps can be employed advantageously. Experimental Method All testing was done at room temperature using a Baldwin universal testing machine. A microformer extensometer was used in conjunction with a micro-former-type stress-strain recorder. All tests were conducted at constant loading rate, the slowest rates being used. This corresponded to 120 lb per min in the 1200 lb full scale range and 300 lb per min in the 6000 lb full scale range. After the rate of loading was set in the elastic range of the material during the early part of the test, no further adjustments were made, allowing the test to proceed at that setting. In the plastic region of the curve above the yield region, strain rates of from 0.002 to 0.006 in. per min were regularly obtained. All experimentation was carried out on specimens machined from the same lot of beryllium, lot No. Y5036BP. Table I shows the chemical analysis as furnished by the supplier, Brush Beryllium Co., as well as the standard specifications to which commercial beryllium is produced. Both 1/4 in. thick hot pressed plate and ½ in. round hot pressed and warm extruded rods were obtained. The history of the material is reported to be as follows: 1—Beryllium metal plates, produced from a standard hot pressed QMV beryllium metal block 4x15x40 in., were cut off and finished machined to 1/4x6x12 in. flat plates. The original hot pressed block was made by hot pressing —200 mesh vacuum cast attri-tioned powder at about 1050°C under vacuum. 2—Beryllium rod was hot pressed and warm extruded. Extrusion billets were machined from the regular hot pressed blocks followed by extrusion at 425°C. The extrusion was done without jacketing, and graphite was used as a lubricant. The rods were then straightened at 720 °C, after which they were annealed at 800°C for 15 min. Both flat tensile specimens and round tensile specimens were tested. The former were machined from the plate stock into standard specimens according to specifications shown in ASTM E8-52T. The nominal cross-section was 0.25x0.500 in. and the gage length was 2 in. The round specimens were

Jan 1, 1956

Discussion * of the paper of H. M. Chance, presented at the butte meeting, august, 1913, and printed in bulletin No. 79, July, 1913, pp. 1315 to 1341. George H. Ashley,+ Washington, d. C.:-Mr. Chance's long practical experience in reporting on coal lands admirably fits him for a discussion of the value of such lands. On behalf of the government geologists, I wish to express my appreciation of Mr. Chance's friendly, constructive criticism of the government method of valuing coal land in the first part of his paper and, at the same time, to reply to some queries he makes. All admit that coal has no " intrinsic "-monetary value, in the sense that a pound of coal of certain chemical and physical characters is worth " intrinsically " so many cents or fractions of a cent. The term has, however, been found very useful as including those natural factors of coal value, among which are its position and location in the earth, that affect its sale price in contrast with the other cost elements involved in the labor and capital necessary in mining, preparing, transporting, and selling the coal (extrinsic factors). Mr. Chance, while recognizing the " dual origin of value," does not offer any better terms. The survey agrees with Mr. Chance in his definition of coal conservation, that it means the fuller utilization of the heat contents of the coal, and the more complete recovery of the coal from the ground. Coal land withdrawals have not been made to keep such lands off the market, but to prevent their acquisition as non-coal lands before they could be classified so as to be disposed of under the proper law. Nor has the pricing of the more valuable coal lands above the minimum been to raise money for the reclamation fund, to which the money goes, but primarily to discourage the alienation, for holding or speculation, of coal lands not intended or needed for development, and, secondarily, to secure to the people the ?unearned increment," which they are certain in any case to be charged.

Jan 11, 1913

By George F. Kunz, Henry S. Washington

The recently discovered occurrence of diamonds near Mur-freesboro, Pike county, Ark., was brought to our attention by Mr. Samuel W. Reyburn (Trustee for Messrs. C. S. Stifft, A. D. Cohn, August Zinsser, Jr., and himself, owners of the property), through whose courtesy we investigated the locality of the deposit. Prospecting with the diamond-drill is now in active progress; but mining operations on a large scale have not yet been ordered. Geology.—The geology as well as the petrography of this interesting locality has been well described by Messrs. J. C. Branner and R. N. Brackett,' but they did not class it as dia-mondiferous, although Branner suggested that it might be. Briefly summarized, the igneous rock in which the diamonds are found is a vitreous peridotite, forming a stock or volcanic neck, which has broken up through the Carboniferous and Cretaceous quartzites and sandstones. After an extensive period of erosion, during which an unknown portion of the neck and pre-

Jan 1, 1909

By F. T. Selleck, H. H. Reamer, B. H. Sage

An experimental investigation was made of the effect of temperature upon the three-phase pressure associated with the propane-water and propene-water systems when hydrates were present. In addition, the characteristics of the propane-propene-water system were established over a limited range of ternperatureo under conditions such that hydrate was formed. The hydrate phase for this system may he a solid solution and the distribution of propane and propene in it is similar to that found in the coexisting hvdrocarhon liquid phase. INTRODUCTION A knowledge of the characteristics of hydrates of the hydrocarborrs encountered in industrial practice is of importance in connection with the design of process equipment. Villardl.1,2 carried out early studies of hydrates, and de Forcrand1 con-sidered the more probable compositions of the hydrates of hydrocarbons. Hammerschnid1 presented information about the propane-water and the isobutane-water systems. Scheffer5 studied the hydrate of hydrogen sulfide in detail, and de For-crand reported on the hydrates of krypton, argon, and xenon.1 Roberts and co-workers1,2 determined the nature of the hydrates formed in the methane-water and ethane-water systems. Carson and Katz10 studied the methane-propane-water, methane-pentane-water, and the methane-hexane-water systems in the four-phase region. The results of this rather extensive investigation indicated that the paraffinic hydrates formed solid solutions. The experimental evidence now available does not Support the existence of hydrates of the pentanes-antl-heavier hydrocarhons but it cannot be stated with certainty that such hydrates are not formed. Stackelherg. 11,12,13 made extensive studies of the crystal structure of paraffinic hydrate; by means of x-ray techniques and found that hydrates poses; a definite structure and composition. The existence of such a Structure does not preclude the firmation of Solid solutions of hydrates in aqueous systems containing two or more hydro-carbon~. Wilcox, Carson and Katz" reviewrd the information on the hydrates of importance in the processing of natural gas and presented data concerning their formation from natural gas. Kobayashi and Katz1' made studies at high pressure of the Hydrate of methane. and Unruh and Katz"' investigated hy-drates in mixtures of carbon rlioxide and methane. Frost and Deaton contributed to the knowledge of the composition of the paraffinic hydrates The irregularities in the experimental results were several times the expected uncertainties. This experience confirms the behavior encountered by other investigators indicating that hydrates tend to occlude water during their formation, thus rendering difficult the direct measoremeut of their composition. Miller and Strong2 investigated a number. of paraffinic hydrates from the standpoint of their possible application to (, the industrial storage of gas. Powel1 studied the effect of solutes upon the decomposition temperature of paraffin hydrates. Marked lowering of the decomposition temperature at a given pressure may he obtained by the use of such additive agents as ethylene glycol, urea. and sodium chloride. APPARATUS AND METHODS Two method* were here employed to study the behavior of hydrates. The first involved a glass capillary within which the hydrocarbons and water were confined over mercury. The second made use of a double-ended weighing bomb technique." The glass capillary equipment has been described elsewhere.'" A schematic drawing of it is presented in Fig. 1, where the arrangement of the agitator and mercury reservoir is shown in some detail. The lower part of the glass capillary, D, was enlarged to afford space within which the fluids used in the investigation could he stored at low pressures after their introduction through the valve. G. The temperature of the capillary was controlled by the circulation of a hydrocarbon oil of low viscosity from the agitated bath, B, through the vacuum jacketed column. C. The pump, A, was employed for the circulation of this oil. A relatively clear view of the capillary tube, D, was obtained through the vacuum jacket. Mercury was introduced into the lower part of the vessel, E, from

Jan 1, 1952

By Paul Pietrokowsky

THE formation of intermediate phases in the solid state reaction of titanium with silicon, germanium. and tin (of subgroup 4B in the periodic table) was the subject of a recent paper.' Further investigation of the system Ti-Sn revealed the presence of a new compound on the titanium-rich side of this phase diagram. Metallographic evidence indicated that this new phase was situated very close to 75 atomic pct Ti. The present work is concerned with the crystal structure of the intermediate phase Ti3Sn. Iodide-process titanium metal, furnished by the New Jersey Zinc Co., was used in this investigation. The metallic tin was received in powder form from Charles Hardy Inc., New York; its purity was 99.80 pct. The titanium rod was machined into small cups 1 cm in diam and about 1.5 cm in height. The tin powder was compacted, melted, and then placed in the titanium cups and alloyed by electric arc melting in a helium atmosphere. The alloys, weighing approximately 8 g, were sealed in evacuated quartz tubes and homogenized at 1030°C for 5 days. This isothermal heat treatment was terminated by a water quench from the soaking temperature. Filings of the alloyed pellets were sealed in evacuated quartz bulbs and quenched from 1030°C into liquid argon. A 14.32 cm Debye Scherrer X-ray camera was used for the powder diffraction study. The copper radiation was filtered. X-ray diffraction data for the compound Ti3Sn are given in Table I. The data were indexed on the basis of a hexagonal lattice. Good agreement between observed and calculated values of the square of the reciprocal interplanar spacings was obtained with the following expression: (1/d)2 = 0.03810 (h2 + hk + k2) + 0.04410 (l2) Unit cell parameters were calculated by the method of least squares from the reflections (20.3), (22.2), (40.1), and (42.1); ao = 5.916 & 0.004A, co = 4.764 ± 0.004A, and co/ao = 0.805. The relatively small size of the unit cell allowed the unambiguous indexing of most of the reflections from planes of large spacing. An inspection of the assigned indices (Table I) reveals the absence of (hk.l) reflections when 1 2n. A systematic absence of this type leads to the space group C 6/mmc or one of its subgroups. Assuming, for a first approximation, a linear increase in the density of titanium with the addition of tin, it follows that there are two stoichiometric molecules of Ti3Sn per unit cell. The density calculated from X-ray measurements is 5.194 g cm-'. At this point it became clear that Ti3Sn might be isomorphous with Mg3Cd. The 6 Ti and 2 Sn atoms were placed in the following positions of space group D4 6h, C 6/mmc: 6Tiin (h): X 2X 1/4; 22;; 1/4;Xx 1/4;x2x3/4; 2x x 3/4; x x 4; with x = 516 2 Sn in (c): 1/3 2/3 1/4; 2/3 1/3 3/4.

Jan 1, 1953

By W. Mckewan, W. M. Fassell

The oxidation rates of copper have been determined at temperatures from 600" to 900°C in oxygen from 14.7 to 400 psi total oxygen pressure. The oxidation rate of copper is unchanged by oxygen pressures within the range studied. The observed data extend Feit-knecht's conclusion concerning the pressure independence of copper from atmospheric pressure to 400 psi. All samples studied in the above-mentioned temperature and pressure range have both Cu2O and CuO present in the oxide film. NUMEROUS papers have been published on the oxidation of copper, some of which have noted the effect of oxygen pressure on the oxidation rate of copper. It must be noted, however, that no data on the oxidation rates of copper at pressure in excess of 1 atm have been reported in the literature. (Le Chatelier¹ reported that a black oxide of silver was formed at 300°C and 15 atm pressure.) This is likewise true for the other metals. This investigation was initiated to obtain experimental oxidation rate constants for pure metals at elevated temperatures and high oxygen pressure. Copper was selected as the first metal since probably more reliable data are available on its oxidation rates and related physical and chemical properties than for any other metal or alloy. As a general summary, the following conclusions appear well established for the oxidation of copper: 1—The oxide coating consists of Cu2O with a superficial coating of CuO providing the ambient oxygen pressure exceeds the equilibrium pressure for the coexistence of Cu2O and CuO.² The following sequence of phases is then Cu/Cu2O/CuO/O2 (gas). The Cu2O consists of large crystals that have no relation to the orientation of the metal crystals, except for a very thin layer adjacent to the metal." The CuO consists of very fine crystals randomly oriented. If the oxygen pressure is below the equilibrium pressure for the coexistence of Cu2O and CuO, the coating consists of Cu,O only. 2—The rate-determining factor in the parabolic oxidation of copper is the diffusion of Cu+ ions through the Cu,O layer.4,6,7 The Cu+ ions are accompanied by electrons to maintain electrical neutrality. The mechanism of the reaction at the Cu2O/CuO interface and the method of growth of the CuO is in some doubt. 3—On copper, there are three reported pressure effects: (a) At pressures below 0.3 mm Hg oxygen pressure, the oxidation rate increases directly with pressure.', ' .Vxygen starvation at the surface may account for this effect. (b) At oxygen pressures from 0.3 to 63 mm, the oxidation rate increases as the 7th root of the oxygen pressure providing the temperature is such that only Cu2O is present in the film. (c) At pressures from above the equilibrium pressure for the coexistence of Cu2O and CuO (varies with temperature) to atmospheric pressure, the oxidation rate is independent of the oxygen pressure.' Equipment In order to determine the oxidation rates of metals in an oxidizing atmosphere at pressures up to 400 psi, the equipment is somewhat different than for low pressure work as is shown in Figs. 1 and 2. A Leeds and Northrup Micromax recording controller (A) is used to control the temperature of the Ni-chrome furnace winding in conjunction with a Micromax electric drive unit. The drive unit adjusts a 20 amp Variac (variable transformer) to control the power input into the Nichrome furnace winding. Due to the "self heating" of the sample by oxidation, frequently encountered in oxidation rate studies, it is essential that the sample temperature be measured independently. This is done by means of a series of six chromel-alumel calibrated thermocouples located spirally around the oxidizing metal sample. Each thermocouple is partially shielded from the direct radiation of the furnace wall by

Jan 1, 1954

By D. E. Moore

The strength of a natural serpentinite gouge was measured at 400°C and an effective pressure of 100 MPa. The strength of the gouge decreased with increasing pore pressure to 50 MPa and then was nearly constant between 50 and 125 MPa. The samples at 50-125 MPa pore pressure slid stably, whereas those at 3-25 MPa pore pressure showed stick-slip behavior. Lengthening the pre-heating time to 72,000 s of samples at 100 MPa pore pressure led to increases in both the strength and the likelihood of sliding unstably. With still longer pre-heating times, the strengths decreased again and sliding once more became stable. The strength of the gouge at 3 MPa pore pressure was unaffected by changes in pre-heating time. A possible explanation for the results is that excess pore pressures are being generated in the gouge, causing the true effective pressure to be lower than the apparent value.

Jan 1, 1984

By H. P. Greenwald

THIs paper brings forward a discussion that was prepared for the meeting of the Coal Division in Chicago in 1938.1 War in Europe less than a year after that meeting, followed by our defense preparations and entry into the conflict, caused general cessation of large-scale experimentation on the subject, and it is best to confine this paper to events in the United States during the five-year period since the preceding paper was written. The views of members of the Coal Division's Committee2 on Rock-dust-ing for 1943 were obtained before this paper was written and the manuscript was reviewed by them. Extent of Rock-dusting Statistics on the use of rock dust in the United States during the years 1930-1933, appearing on page 97 of Volume 139 of the Transactions are extended in Table I herein through the year 1941. The results through 1933 did not appear encouraging, but there has been improve-ment since that date. It has always been true that the larger operations were the ones that used rock dust. In 1941 only 10 per cent of the mines in the country used rock dust, but they produced 57 per cent of the coal, employed just under 50 per cent of the miners, and accounted for 52 per cent of the man-hours. Unfortunately, collection and compilation of these statistics are slow procedures, and figures dealing with the tremendous war expansion of the industry are not likely to be available for a year or more. In 1941 the five leading states in regard to percentage of man-hours worked in mines using rock dust were: Utah, 92.1; Wyoming, 79.3; Alabama, 77.4; New Mexico, 72.5; West Virginia, 65.3. The first four states were the same as in 1933, but West Virginia displaced Washington in fifth place. On the basis of pounds of rock dust used per ton of coal, the five leading states in

Jan 1, 1944

By H. P. Greenwald

THIs paper brings forward a discussion that was prepared for the meeting of the Coal Division in Chicago in 1938.1 War in Europe less than a year after that meeting, followed by our defense preparations and entry into the conflict, caused general cessation of large-scale experimentation on the subject, and it is best to confine this paper to events in the United States during the five-year period since the preceding paper was written. The views of members of the Coal Division's Committee2 on Rock-dust-ing for 1943 were obtained before this paper was written and the manuscript was reviewed by them. Extent of Rock-dusting Statistics on the use of rock dust in the United States during the years 1930-1933, appearing on page 97 of Volume 139 of the Transactions are extended in Table I herein through the year 1941. The results through 1933 did not appear encouraging, but there has been improve-ment since that date. It has always been true that the larger operations were the ones that used rock dust. In 1941 only 10 per cent of the mines in the country used rock dust, but they produced 57 per cent of the coal, employed just under 50 per cent of the miners, and accounted for 52 per cent of the man-hours. Unfortunately, collection and compilation of these statistics are slow procedures, and figures dealing with the tremendous war expansion of the industry are not likely to be available for a year or more. In 1941 the five leading states in regard to percentage of man-hours worked in mines using rock dust were: Utah, 92.1; Wyoming, 79.3; Alabama, 77.4; New Mexico, 72.5; West Virginia, 65.3. The first four states were the same as in 1933, but West Virginia displaced Washington in fifth place. On the basis of pounds of rock dust used per ton of coal, the five leading states in

Jan 1, 1944