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By R. W. Raymond

The death of Louis Janin, which took place Mar. 6, 1914, at Santa Barbara, terminated the earthly career of almost the last survivor, and one of the most illustrious members, of that group of American mining engineers and metallurgists who, in the last quarter of the nineteenth century, directed the development of the mineral resources of the Pacific slope. Louis Janin was born in 1836 at New Orleans. His grandfather, an officer in the French army, had emigrated to this country, with his family, at or before the outbreak of the French revolution. His father became an

Jan 1, 1915

By W. W. Stephens, W. J. Kroll, H. P. Holmes

THE only two methods for producing commercial quantities of malleable zirconium, up to now, have been using magnesium reduction of the anhydrous chloride under a neutral gas, and using purification of raw zirconium by the iodide dissociation method on a hot filament. The purity of the metal obtained by the latter process is about the same as that resulting from the chloride reduction, with the exception of the oxygen content, which may be about 0.05 pct lower in the iodide metal. Even traces of oxygen have a strong hardening effect on zirconium. Since, in the iodide process, the impurities, Si, Al, Fe, Ni, and Mg in the raw zirconium used, are carried over, it would appear uneconomical to use this method of refining solely to eliminate the traces of oxygen, unless very soft metal is desired. One important step to improve the iodide method, namely, dissociating pure iodide made from carbide and recycling the iodine, which would change this refining process into a method for extracting zirconium from the ore, has not yet been made. The Bureau of Mines, by using the chloride reduction, wanted to produce quantities of a reasonably pure and malleable metal at low cost for large-scale industrial use. This aim has been achieved, and a pilot plant permitting production of 600 lb of malleable zirconium per week will be described (fig. 1). Briefly, the Bureau of Mines process consists of reducing purified gaseous anhydrous zirconium chloride with fused magnesium under a noble-gas atmosphere. The reaction product, magnesium chloride, and any excess magnesium metal present are removed from the sponge zirconium in the next step by fusion and evaporation in a good vacuum at about 925°C. In this process, care is taken to keep air out of contact with the hot metal, which otherwise would contaminate the product with oxygen and nitrogen. Both these impurities embrittle zirconium even when present in an amount as low as 0.1 pct. A number of previous reports1-3 describe the method and the various improvements that finally led to a workable process. The major steps made were the production of large quantities of carbide, which is the raw material for producing the chloride, its chlorination with reasonable efficiencies, and the elimination of iron trichloride contained in the raw chloride, as well as that of the zirconium oxide which is always present in this product. The physical nature of the anhydrous chloride, which sublimes at 331°C at atmospheric pressure and melts at 420°C under a pressure of 25 atm, made it necessary to provide a special safety device on the purification and reduction vessels in the form of a lead-alloy seal, permitting escape of excess gases if pressure tended to build up. The main difficulties encountered in the reduction and in the following step, salt separation in a vacuum at elevated temperature, were caused by the material from which the reaction pot was constructed—iron. This metal reacts with zirconium at about 940°C with formation of a eutectic. The last step, salt separation by evaporation of the magnesium and magnesium chloride in a vacuum, is quite unconventional and has not been used before on such a scale. It is only due to the improved construction of high-vacuum pumps, especially oil-diffusion pumps, that such a method could be used. The various steps of the Bureau of Mines process, as described in the general outline above, may be summarized as follows: (1) production of the carbide, (2) chlorination of the carbide, (3) purification of the raw chloride, (4) reduction of the pure chloride with fused magnesium, (5) separation of excess magnesium and magnesium chloride in vacuum at elevated temperature, and (6) melting of the sponge obtained. Production of Carbide The arc furnace, described in a previous report,' was improved both to reduce the graphite consumption caused by the burning of the bottom plates and to concentrate the heat in order to obtain better power efficiency. This was achieved by providing the bottom with graphite plates entirely embedded in refractory bricks, the contact with the current being made with three water-cooled copper plugs. Figs. 2 and 3 show the arrangement. The crucible, made

Jan 1, 1951

By John H. Hearding

Induction heating, together with automatically controlled tempering and hardening is giving Oliver faster and more accurate bit sharpening, while experiments with bit taper promise to offer increased footage per bit.

Jan 10, 1953

E. E. THUM,* Salt Lake City, Utah (written discussion?).-While the present paper is confined exclusively to the microstructure of fusion welds, it may be of interest to draw attention to certain appearances existing in resistance welds such as spot or butt-welded joints produced by the Thomson process. For instance, a butt weld between two pieces of carbon tool steel (carbon about 0.90 per cent.) will show concentric ellipsoids of the various materials from pearlite to martensite. The surfaces of demarcation are quite well defined, the center of the ellipsoid being at the intersection of the axis of the piece and the plane of the weld. Often these unannealed welds show a troostitic center; evidently this core was not quenched as rapidly as the surrounding shell. Such specimens are beautiful samples for instruction purposes. An annealed butt weld of this kind will show a very well defined central ellipsoid of decarburized, materials. It is interesting to consider the reason why this change takes place. It must be understood that the heat is on the metal for a very short time, possibly 30 sec. It is therefore evident that the decarburization, or migration, of the carbon takes place with extreme rapidity. Since no blowholes are evident in a well-made butt weld, the deoxidizing air and the products of combustion must migrate with the highest speed; second, the carbon might migrate back into the stock; or, last, a large proportion of the pearlite may be extruded with the hot metal, which forms a fin at the plane of weld. Examining these possibilities in detail, it is not probable that such deep-seated decarburization, extending with maximum effect to the very center of a 2-in. round bar, is done by reaction with the oxygen of the air. This would postulate entrance of oxygen and egress of carbon oxides in large quantity without leaving behind traces in the form of oxides or

Jan 5, 1919

The annual report f the Secretary of the Navy for the fiscal year, ending June 30, 1917, but including operations and recommendations up to Dec. 1 of that year, contains the following remark about the activities of the Naval Consulting Board. The members of the Institute who are members f this Board are William L. Saunders, Benjamin B. Thayer, Thomas A. Edison, Thomas Robins, Lawrence Addicks, Joseph W. Richards, W. R. Whitney, assisted by 47 other members f the Institute, in the capacity of associate members of the Naval Consulting Board. During the year, the work of this board, organized and approved by Congress in 1915, has increased very materially in importance and volume, its meetings have been frequent and the work of its individual members has been such in some cases as to occupy almost their entire time in the service of the Government. Some time before the active entry of this country into war the board called a special meeting to which were invited some 50 of the leading scientists and industrial managers, whose special study fitted them to advise on the methods of meeting the

Jan 2, 1918

By Barry S. Epstein

Financing the acquisition of a going coal mine operation has not had the exposure other finance-oriented projects have had. Therefore, C.I.T. feels that coal mining people and financial people should improve their understanding of the factors involved in this important type of acquisition. The discussion consists of two major subjects: analysis of the acquisition of the property, and sources and terms of funding the acquisition. Source and Terms of Funding There is a need to keep the competent medium-sized independent operator in the coal business, especially in these times of energy shortage. The creation of a resale market for coal mines encourages new investment in the coal mining business by medium-sized operators and their financial backers. Who provides debt and equity financing to acquire going coal mine operations and on what terms?

Jan 9, 1975

By A. E. Jenkins, A. Jostsons

Isothermal sections of the Ti-0-H phase diagvam at 600°, 700°, and 800°C have been constructed from equilibrium hydrogen pressure measurements over a range of Ti-0-H alloys containing up to 34 at. pct 0. Oxygen reduces the hydrogen solubility at fixed hydrogen pressure but increases the terminal solubility in the a solid solutions at the a/(a + P) phase boundary. Metal-lographic studies of alloys annealed below the eutectoid temperature show that oxygen also increases the ter-ninal solubility of hydrogen in the a solid solution in equilibrium with the hydride phase. The effect of oxygen on hydrogen solubility is discussed in terms of the electronic and geometric structure of interstitial solid solutions. THE isothermal solubility of hydrogen in a Ti-0 alloys at 800°C has been measured by Hepworth and ~chuhmann' who subsequently used ternary Gibbs-Duhem integrations to calculate oxygen activities in binary Ti-0 alloys. The present study aims to extend Hepworth and Schuhmann's measurements to alloys richer in oxygen and to a range of temperatures. This paper presents the results of hydrogen equilibrium pressure/concentration measurements in Ti-0 alloys as well as observations on the effect of oxygen on the terminal solubility of hydrogen in a titanium. The thermodynamic properties of binary Ti-0 alloys, derived from these measurements, will be published separately.' EXPERIMENTAL METHODS Specimen Preparation. Ti-0 alloys were prepared from iodide-refined titanium and titanium dioxide obtained by hydrolysis of redistilled titanium tetrachlo- ride. Specimens containing up to 16 at. pct 0 were prepared by electromagnetic levitation3 whereas a conventional tungsten arc furnace with a water-cooled copper hearth was used to melt oxygen-rich alloys. The specimen homogeneity was indicated by the constancy of lattice parameters of samples from various parts of the ingot as well as by the sharpness of the reflections on X-ray powder patterns. Oxygen-rich specimens in the composition range (20 to 34 at. pct), where ordering has been ~bserved,~ were annealed for 300 hr at 600°C prior to use in hydrogen solubility measurements. Apparatus. The hydrogen pressure/concentration measurements were made with a modified Sieverts apparatus shown diagrammatically in Fig. 1. Specimens were placed in a clear silica tube and impurity pickup by direct reaction with silica was prevented by lining the heated end of the silica tube with thin molybdenum sheet. A double silica tube was required to eliminate loss of hydrogen by diffusion through silica at high temperatures and high hydrogen pressures, the space between the tubes being maintained at a hydrogen pressure equal to that above the specimen. Hydrogen was purified by diffusion through a Ag-Pd tube.= Hydrogen pressures were measured with a mercury McLeod gage in the range 0.001 to 4 Torr

Jan 1, 1968

By H Pray, H. W. Russell, Paul D. MILLER

It is known that austenitic chromium-nickel steels that have free carbide in the grain boundaries are subject to intergranu-lar corrosion. It is difficult to detect such a susceptible condition in a fabricated article because present test methods require a sample section for examination and in most cases this is difficult to obtain. The question of the nature and prevention of intergranular corrosion in austenitic stainless steels has been ably discussed by Bain and co-workers1-3 and by other investigator4-10 The present methods of study subject samples to corrosive conditions in such reagents as the Strauss solution, a mixture of copper sulphate and sulphuric acid. Such tests usually require at least 72 hr. to run. Various methods of measuring the degree of sensitization have been employed, such as the measurement of electrical resistivity, magnetic measuremerits, measurement of the degree of cracking produced on bending over a malldrel, and microscopic studies. The detection of carbides at the grain boundaries by metallographic polishing and etching methods is tedious and requires a skilled operator. A recent report on such methods of carbide detection is given by the American Society for Testing Materials Subcommittee VI of Committee A.-1011 and by Arness.12 The present investigation was undertaken to develop a simple test procedure for detecting carbide precipitation or susceptibility to intergranular corrosion. The test is designed for use in the plant and for the testing of fabricated structures. Carbide precipitation, the factor leading to susceptibility to corrosion, is produced by heating the alloy in the temperature range 800° to 1600°F., as in welding, in improper annealing or in service where such temperatures are met. The connection between such precipitation and susceptibility to corrosion has been thoroughly discussed, as has been the use of stabilizing addition elements to prevent precipitation. Experimental Method A small area of the steel under test is subjected to an anodic treatment in a cell that can be 'lamped Onto a a Or an actual structure. The cell and electrical circuit used are illustrated in Fig. I. The cell C is lead, joined to the steel plate D and insulated from it by a short piece of rubber tubing E. The cell is forced tightly against the steel plate by a spring Or clamping device. The seal formed by the rubber against the steel plate is sufficient to retain the liquid bath inside the cell. The spot treated can be made any shape desired, depending on the shape of the rubber gasket. The cell illustrated polishes a circular spot about 3/8- diameter' The bath consists of 60 per cent (by weight) sulphuric acid to which is added 5 ml. per liter of Glycyrrhiza extract (U.S.P.). The cell requires about 2 to 2.5

Jan 1, 1941

By H. W. Russell, H Pray, Paul D. MILLER

It is known that austenitic chromium-nickel steels that have free carbide in the grain boundaries are subject to intergranu-lar corrosion. It is difficult to detect such a susceptible condition in a fabricated article because present test methods require a sample section for examination and in most cases this is difficult to obtain. The question of the nature and prevention of intergranular corrosion in austenitic stainless steels has been ably discussed by Bain and co-workers1-3 and by other investigator4-10 The present methods of study subject samples to corrosive conditions in such reagents as the Strauss solution, a mixture of copper sulphate and sulphuric acid. Such tests usually require at least 72 hr. to run. Various methods of measuring the degree of sensitization have been employed, such as the measurement of electrical resistivity, magnetic measuremerits, measurement of the degree of cracking produced on bending over a malldrel, and microscopic studies. The detection of carbides at the grain boundaries by metallographic polishing and etching methods is tedious and requires a skilled operator. A recent report on such methods of carbide detection is given by the American Society for Testing Materials Subcommittee VI of Committee A.-1011 and by Arness.12 The present investigation was undertaken to develop a simple test procedure for detecting carbide precipitation or susceptibility to intergranular corrosion. The test is designed for use in the plant and for the testing of fabricated structures. Carbide precipitation, the factor leading to susceptibility to corrosion, is produced by heating the alloy in the temperature range 800° to 1600°F., as in welding, in improper annealing or in service where such temperatures are met. The connection between such precipitation and susceptibility to corrosion has been thoroughly discussed, as has been the use of stabilizing addition elements to prevent precipitation. Experimental Method A small area of the steel under test is subjected to an anodic treatment in a cell that can be 'lamped Onto a a Or an actual structure. The cell and electrical circuit used are illustrated in Fig. I. The cell C is lead, joined to the steel plate D and insulated from it by a short piece of rubber tubing E. The cell is forced tightly against the steel plate by a spring Or clamping device. The seal formed by the rubber against the steel plate is sufficient to retain the liquid bath inside the cell. The spot treated can be made any shape desired, depending on the shape of the rubber gasket. The cell illustrated polishes a circular spot about 3/8- diameter' The bath consists of 60 per cent (by weight) sulphuric acid to which is added 5 ml. per liter of Glycyrrhiza extract (U.S.P.). The cell requires about 2 to 2.5

Jan 1, 1941

POSITIONS VACANT (Under this heading will be published notes sent to the Secretary of the Institute by members or other persons.) Position open as assistant superintendent at a steel plant. Practical experience in the manufacture of crucible and open-hearth steel and heat treatment of steel and alloy steels required. This position offers an excellent future. No. 9. A company in Virginia desires a man with experience in Western mines to act as superintendent of its pyrite mine. No. 15. Position open as instructor at a University in Middle West to teach the mechanical side of mining, such as hoisting, haulage, drilling, and mine surveying. Salary, $1,500 to $1,800. No. 16. Experienced amalgamator wanted at a mill in Ivory Coast, Africa. An American speaking French preferred. No. 18.

Jan 5, 1914

By H. W. Russell, Paul D. MILLER

IT is known that austenitic chromium-nickel steels that have free carbide in the grain boundaries are subject to intergranular corrosion. It is difficult to detect such a susceptible condition in a fabricated article because present test methods require a sample section for examination and in most cases this is difficult to obtain. The question of the nature and prevention of intergranular corrosion in austenitic stainless steels have been ably discussed by Bain and co-workers1-3 and by other investigators.4-10 The present methods of study subject samples to corrosive conditions in such reagents as the Strauss solution, a. mixture of copper sulphate and sulphuric acid. Such tests usually require at least 72 hr. to run. Various methods of measuring the degree of sensitization have been employed, such as the measurement of electrical resistivity, magnetic measurements, measurement of the degree of cracking produced on bending over a mandrel, and microscopic studies. The detection of carbides at the grain boundaries by metallographic polishing and etching methods is tedious and requires a skilled operator. A recent report on such methods of carbide detection is given by the American Society for Testing Materials Subcommittee VI of Committee A-10 11 and by Arness.12 The present investigation was undertaken to develop a simple test procedure for detecting carbide precipitation or susceptibility to intergranular corrosion. The test is designed for use in the plant and for the testing of fabricated structures. Carbide precipitation, the factor leading to susceptibility to corrosion, is produced by heating the alloy in the temperature range 800° to 1600°F., as in welding, in improper annealing or in service where such temperatures are met. The connection between such precipitation and susceptibility to corrosion has been thoroughly discussed, as has been the use of stabilizing addition elements to prevent precipitation. EXPERIMENTAL METHOD A small area of the steel under test is subjected to an anodic treatment in a cell that can be clamped onto a sample or an actual structure. The cell and electrical circuit used are illustrated in Fig. I. The cell C is lead, joined to the steel plate D and insulated from it by a short piece of rubber tubing E. The cell is forced tightly against the steel plate by a spring or clamping device. The seal formed by the rubber against the steel plate is sufficient to retain the liquid bath inside the cell. The spot treated can be made any shape desired, depending on the shape of the rubber gasket. The cell illustrated polishes a circular spot about 3/8-in. diameter. The bath consists of 60 per cent (by weight) sulphuric acid to which is added 5 ml. per liter of Glycyrrhiza extract (U.S.P.). The cell requires about 2 to 2.5

Jan 1, 1941

By Arthur H. Leigh

Anode mud, the residual material collected from the bottom of the electrolytic cells during the refining of copper is leached, roasted, fire-refined and cast into Dore1 metal anodes. Dore1 metal is a gold-silver-copper alloy containing 80 percent silver. The metal is processed electrolytically using the Moebius system to refine silver and separate gold, platinum and palladium. The Moebius cell cathodes receive a deposit of silver crystals which are melted and cast into 1000 ounce silver bars with 999 Fine minimum purity. Gold mud is collected in fabric bags and cast into gold anodes for further refining in the Wohlwill cells. Wohlwill cells are unique in that gold, the noble metal, can be put into solution electrolytically without the use of aqua regia. Gold is collected on high purity gold foil cathodes and cast into 400 ounce bull ion with 999.7 Fine minimum purity. Platinum and palladium remain in the electrolyte progressively increasing in concentration and are finally separated and purified by precipitation.

Jan 1, 1973

By John A. Meech, J. G. Paterson

Activated carbon is a strong adsorbent for amyl xanthate, capable of removing from solution up to a quarter of its own weight in xanthate. In selective flotation system where depression is unstable, separation efficiency increases with activated carbon additions. The improvements observed are brought about by two mechanisms. First, by removing stripped and residual collector ions from solution, competition between depressant and xanthate is reduced and depression is stabilized. In addition, the texture of the froth phase at high pine oil concentrations is modified by activated carbon such that better drainage between the air bubbles takes place, alleviating the mechanical entrapment of depressed mineral particles. In treating a bulk copper/lead concentrate produced from GECO ore, selectively between galena and chalcopyrite is increased when activated carbon is used. Although the rate of flotation of galena is marginally lowered by activated carbon, a small extension in the duration of flotation allows the lead recovery to increase by 19% at the same recovery of copper. An addition rate of 0.75 kg/ton (1.5 lb/st) of bulk concentrate is suggested as optimum from this testwork. However, the actual level used in the mill is dependent upon the residual concentrations of collector and frother in the bulk concentrate pulp.

Jan 1, 1979

* A complete magnetic picture of the Mesabi range is now available for the first time with the release of 21 additional maps based on the aeromagnetic survey of 30,000 square miles made jointly by the USGS and the Minnesota Geological Survey. A potential iron formation with a magnetic pattern remarkably like that of the Mesabi iron range lies buried beneath the glacial drift in a wide belt extending some 30 miles across the northwest corner of Itasca County in north central Minnesota. Identification of three new uranium minerals by the USGS was recently announced. The new minerals, andersonite, swartzite, and bayleyite are, respectively, hydrous uranyl carbonates of magnesium, of sodium and calcium, and of calcium and magnesium. They were first observed by Charles A. Anderson, Survey geologist, in a coating on gypsum on the 300-ft level of the Hillside mine, Yavapai County, Arizona. International Minerals and Chemical Corp. has announced a $4,000,000 expansion and development program in the Polk County phosphate fields in Florida, Plants for the manufacture of multiple superphosphate and phosphate chemicals including dicalcium p osphate for animal feed and chemical purposes, and a sulphuric acid are planned. Office building, machine shop, warehouse, and laboratory are also scheduled for erection. A new type of tramp iron detector is being used on the conveyor belt feeder at the South Agnew stripping operation. It is made of an alloy of aluminum, nickel and cobalt and does not have any electric coils. The alloy, known as Alnico, is remarkable for the permanence and intensity of the magnetism which it retains. The detector was made by Dings Magnetic Separator Co. and it is probable that Alnico will be used in magnetic separators. The American Society of Engineering Education estimates that unless the percentage of high school graduates entering engineering colleges is increased, there is a strong possibility that instead of a large surplus of engineering graduates, which has been propehsied rather widely, there will soon be fewer engineering graduates available than are needed annually by our national economy. This conclusion is reached from a survey that shows that engineering enrollments are only slightly higher than prewar whereas industrial expansion is increasing the need for engineers. * The natural resources of Korea are being investigated under ECA sponsorship. E.J. Longyear has just embarked 8 crews for that country; two drills are scheduled for base metal search while six are slated for development of coal reserves. An innovation in the development work in the iron country has been the adoption of the Drill-Mobile, jumbo-mounted drills on rubber-tired carriage, by Cleveland-Cliffs at the Mather A and B mines. The machine is being used to cut stations in the new Mathed B shaft and for driving development headings at the Mather A.

Jan 5, 1950

By R. P. Smith

The carbon content of a number of alloys ranging (before carburitation) from purified iron to purified cobalt was determined for fixed activities of carbon by equilibration with each of six CO-CO2 atmosphere at 1000°C. At fixed carbon activity, the carbon content decreases continuously with increasing cobalt content. For concentrations of 0 to 50 at. pct Co the results can be expressed by a linear interaction equation of the type In y2 = 7.76n2/(n1+n3)+ 2.30 n3/(n1+n3) where y2 is the activity coefficient of carbon (standard state such that y2— 1 as n2 — 0 in the Fe-C binary) and n1, n2, and n3 are the number of atoms of iron, carbon, and cobalt per unit weight of alloy. The results are also given in terms of the a functions. In the same concentration range, the results are in accord with the regular solution theory of Alcock and Richardson. THE carbon content of Fe-Si, Fe-Mn, and Fe-Ni alloys at fixed activities of carbon has been reported previously.'-, The present work extends R. P. SMITH, Member AIME, is Research Chemist, E. C. Bain Laboratory for Fundamental Research, United States Steel Corp., Research Center, Monroeville, Pa. these measurements to a series of Fe-Co alloys. These alloys, like the Fe-Ni alloys, are fcc ("aus-tenitic") over the entire range of composition at 1000°C. EXPERIMENTAL PROCEDURE The alloys were made from electrolytic cobalt and Plast-Iron in a small vacuum-melting furnace. A small amount of graphite was added to each melt to keep the oxygen content low. The ingots were analyzed for iron and carbon: the amount of cobalt was obtained by difference. Analysis of the top and bottom of the ingots indicated that they were uniform in alloy content. Except for the pure cobalt the ingots were hot-rolled to approximately 0.15 cm thickness, cleaned by sandblasting, then cold-rolled to about 0.045 cm. We were not successful in cold rolling the pure cobalt; therefore it was hot-rolled to the final thickness. The last traces of surface oxide were removed by acid pickel, then the samples were treated in a hydrogen-2 pct water vapor mixture at 1100°C to remove carbon and most of the oxygen. The carburizing procedure was similar to that previously described.1,2,4 The alloys in the form of strips about 1.7 cm wide, 7.5 cm long, and 0.04 cm thick, together with a similar specimen of purified iron, were equilibrated with each of six CO-CO2 mixtures of fixed composition, then quenched in the

Jan 1, 1965

By Robert P. Burrows

Discussion of the paper of R. P. Burrows, presented `at the New York meeting, February, 1916, and printed in Bulletin No. 107, November, 1915, pp. 2237 to 2245. EDWIN M. CHANCE, Wilkes-Barre, Pa.-I have been very much interested in the comprehensive and able discussion of the important topic of mine lighting just given by Mr. Burrows, especially as I know by common report Mr. Burrows' ability and his close touch with the development of the electric mine lamp, and its use in mines in connection with a portable electric lamp. It is regrettable that Mr: Burrows was not able to acquaint himself more closely with the cost of mine illumination, the actual cost, as produced by a portable light as carried by miners, whether a flame safety lamp or an open light. Had he been able to acquaint himself more closely with these data, he perhaps would not have arrived at some of the conclusions which he has presented to us in his paper. For example, we find Mr. Burrows advises that the open torch is by far the cheapest source of illumination, as produced by a portable light. I am very sure that is not the fact. The cost of miners' oil varies from about 25.c. a gallon to 90b. a gallon. The various States have passed laws from time to time rendering it mandatory that the miner shall use, whether he is willing or not, a so-called better or higher grade of burning oil. These laws have entailed the use of an oil so expensive that the use of the oil torch has become practically impossible, and the acetylene or carbide miners' lamp has largely taken its place. I have evolved a few figures showing the relative efficiency and usefulness of the open oil torch and the acetylene miners' lamp. For example, the acetylene miners' lamp consumes or burns 4 liters of acetylene per hour, or 0.14 cu. ft.; the oxygen consumed is 10 liters, or 0.35 cu. ft. per hour; air consumed, 50 liters, or 1.76 cu. ft. per hour; black-damp produced, 40 liters, or 1.41 cu. ft. per hour; air rendered extinctive to the acetylene flame, 112 liters, or 3.95 cu. ft. per hour; carbide con- sumed, 13 g. per hour. The open oil torch, on the other hand, burns about 20 g. of oil per hour; the oxygen consumed is 48 liters, or 1.69 cu. ft. per. hour; air consumed, 240 liters, or 8.47 cu. ft. per hour; blackdamp produced, 191 liters, or 6.73 cu. ft. per hour; air rendered extinctive to oil flame is 1,413 liters, or 49.92 cu. ft. per hour.

Jan 5, 1916

The Joint Economic Committee's subcommittee on international payments and exchange has recommended that, following international monetary reforms, the law which prohibits private possession of gold by American citizens be repealed. The subcommittee recommendation called for reforms to enhance the role of special drawing rights in international monetary affairs and downgrade the role of gold. Special drawing rights, also known as "paper gold", are on artificial reserve with the International Monetary Fund (IMF) which distributes them to member nations in proportion to their economic importance in the world economy. The special drawing rights are then used to settle debts between nations in the same manner as gold or currency. The subcommittee said that under the reforms now being discussed special drawing rights would be acceptable in lieu of gold among the member countries of the IMF.

Jan 1, 1973

By E. J. Dulis, G. V. Smith

AS reported several years ago,' nitrogen may be taken up from the atmosphere by austenitic Cr-Ni steels during creep or creep-rupture tests. This was indicated by chemical analysis and by the appearance of a new microstructural phase, or phases, tentatively identified as chromium nitride (S), at the surface or at the intergranular cracks associated with fracture. The nitrogen pickup was observed to be dependent on time, temperature, and deformation. In a more recent investigation, a sample was obtained in which there was sufficient of the precipitate to suggest that it could be readily identified by X-ray diffraction. This sample had been taken from a 1/4 in. diam creep-rupture specimen of annealed, type 304L stainless steel of the following initial composition: C, 0.03 pct; Mn, 0.65; P, 0.010; S, 0.019; Si, 0.54; Cr, 19.50; Ni, 12.02; N, 0.031; and Al, 0.005. The specimen had ruptured after 10,470 hr at 1500°F (2000 psi). In this case nitrides were distributed across the whole section of the sample, Fig. 1. The precipitate occurred both at the grain boundaries and within the grains; the latter precipitate had in some cases the appearance of pearl-ite, and in others was distinctly Widmanstatten. Chemical analysis of the sample after test showed 0.64 pct "soluble" nitrogen (soluble in 1:1 hydrochloric acid: water) and 0.18 pct "insoluble7' nitrogen (insoluble in the hydrochloric acid solution but dissolved by fuming sulphuric acid). For identification of the precipitate by X-ray diffraction, the matrix in the surface layer of the specimen was dissolved by prolonged attack in an alcoholic solution of picric and hydrochloric acids. The appearance of the specimen surface after such etching is shown in Fig. 1c. The diffraction pattern of the surface-concentrated precipitate was obtained with a recording spectrometer in both the forward and back-reflection regions (the latter by adapting a special fixture to the conventional X-ray unit). The observed X-ray diffraction lines, Table I, show the presence of Cr,N and CrN; the agreement with interplanar spacings calculated from reported data2,3 is quite good. Since it has been suggested' that CrN dissolves only in concentrated sulphuric acid, whereas Cr2N dissolves in dilute hydrochloric or sulphuric acids, an effort was made to distinguish between the two nitrides. This proved possible, inasmuch as etching in a dilute solution of hydrochloric acid gave a sample in which microscopic examination showed that much of the Widmanstatten-pearlitic precipitate within the grains had been eaten out, leaving the grain boundary precipitate in relief, and which, when examined by X-ray diffrac-

Jan 1, 1953

By P. Chiotti, G. R. Kilp

IN the study of zinc-zirconium1 and zinc-uranium2 systems, vapor-pressure measurements were made in order to establish the equilibrium phase diagrams for a pressure of 1 atm. In each of these systems, only zinc has an appreciable vapor pressure over the temperature range investigated. The zinc pressure was measured over a sufficiently wide temperature and composition range to permit calculation of the standard free energy, enthalpy, and entropy of formation for the compounds ZrZn, ZrZn2, ZrZn3, ZrZn6, ZrZn14 , and U2Zn17. In these calculations the compounds were treated as line compounds. Although the exact composition range was not determined, metallographic and thermal data indicate that the solubility range for these compounds is small. It is to be noted that the compound initially reported to correspond to the formula UZn9, 2 has been shown by the crystal structure work of Makarov and vinogradov3 to correspond to the formula U2Zn17,. The crystal structure is similar to that for the compounds Th2M17, investigated by Florio,4 et al; here M represents iron, cobalt, or nickel. Therefore, thermodynamic calculations are based on the formpla U2Zn17 EXPERIMENTAL The dew-point method employed to measure the vapor pressure of zinc over uranium-zinc alloys has been described previously.2 The same procedure and apparatus were used in measuring the zinc pressure over zinc-zirconium alloys. In the case of alloys in the two-phase region consisting of a zirconium and the compound ZrZn, the Knudsen effusion method was employed to obtain a few values in the temperature range 600" to 560°C. In most cases, tantalum crucibles were used to contain the zirconium alloys. THERMODYNAMIC PROPERTIES OFU2Zn17 A least-squares treatment of the vapor-pressure data obtained for 35 and 65 wt pct U alloys in the temperature range 650° to 940°C gave lOg10PAtm = 7,713/T + 6.33 Here, as in following equations, T represents degrees kelvin and P represents the zinc vapor pressure in atmospheres. The probable errors for the two constants were calculated to be 60.68 and 0.0563, respectively. This relation represents the equilibrium dissociation pressure for the reaction U2Zn17 (s) - 2U(s) + 17Zn(v) The solubility of zinc in solid uranium is negligible and the only additional information required to calculate the free energy of formation of U2Zn17 is the free energy of vaporization of pure zinc. K. K. Kelley5 gives the relations, AF°= 30,902 + 6.03Tlog T + 0.275 X 10-3T2 - 45.03T

Jan 1, 1961

By H. H. Podgurski, J. C. M. Li, Y. T. Chou, F. N. Davis, R. A. Oriani

When an Fe-2 pct A1 alloy is nitrogemted at 500ºC with a gus tnixture (NH3-H2) in which the nitrogen activity has been kept Lou] enough to avoid the formation of iron nitride, a two-phase alloy is generuled which consists of AlN particles and a ferrite phase cotaining a heavy network of dislocations. The amount of nitrogen contained in such an alloy, when equilibrated with the nitrogenating atmosphere, far exceeds both that needed to satisfy the normal solution requirements of a Fe and that needed to convert all of the aluninuwi to AlN. This excess nitrogen is accounted for as being trapped on dislocations, adsorbed at the ferrite -AlN interface, and as an en-Iuznced lattice solubility in strained ferrite. This excessive uptake of nitrogen had previously been attribuled by other investigators to the formation of a nonstoichiornetric aluminum nitride. Isotope exchange experiments revealed various amomts of exchargeable N14 present in the originally nitrided samples that could not be removed by reduction with HS at 500ºC. This exchangeable nitrogen has been identified us that bound to the AlN -ferrite interface. Estimates of inter facial areas in alloys containing -3 pct by weight of A1N are as high as 10 sq m per g of alloy. ThE first1 of this series of papers described the experiments forming the basis for the elucidation of the mechanism of the formation of aluminum nitride particles within an Fe-A1 alloy. It was found that not only are dislocations necessary for the nucleation of the AlN particles but also the nitriding reaction in turn produces a dense network of dislocations in the ferrite matrix. It was also observed that nitrogen in excess of that needed for the formation of stoichiometric AIN is taken up by the alloy without the formation of an iron nitride. The present paper is an analysis of the excess nitrogen sorbed by the nitrided Fe-A1 alloy which considers the structure generated by the formation of the aluminum nitride particles. Because of the high density of dislocations, this system has proved to be quite useful in studying nitrogen-dislocation interactions. Wriedt and Darken2 have already reported such studies in a cold-worked ferritic steel. EXPERIMENTAL Nitrogen Sorption. The specimens of this alloy were cold worked (50 pct reduction) to 0.011 in. thickness and chemically cleaned in a 2:1 concentrated phosphoric acid-50 pct hydrogen peroxide solution before nitrogenation. The flowing nitrogenating atmosphere (11 pct NH3-89 pct H2) was established before the ni- trogenating temperature was reached. The same gravimetric and gas-flow equipment described in an earlier paper1 was also used in this investigation. Changes in nitrogen concentration were followed gravimetrically when establishing the isotherms. In the isotope exchange experiments, concentration changes were followed volumetrically. In some instances chemical analyses (Kjeldahl method) were used to check for material balances in both the gravimetric and volumetric procedures. Our objective was to obtain reversible nitrogen sorption isotherms for alloys equilibrated with NH3-H2 gas mixtures over a large range of nitrogen activity* and temperature. The *Defined as equal to PN H /P3/2 ,where P corresponds to partial pressure in atmospheres. Actually the nitrogen activity, aN, in the alloy equals K PNH3 /p3/2H2, where K is the equilibrium constant for the reaction NH3 = N + 3/2H2. upper limit for nitrogen activity was below that which would produce iron nitride; for reasons which will become apparent later, most of the sorption studies were made in the temperature range between 400" and 500'C. The alloy sample studied most extensively in this investigation was given a series of successive reductions (100 pct H2) and nitrogenating treatments at 500°C to attain a stabilized structure. Presumably some dislocations were lost during these treatments. Throughout most of the sorption studies, temperature was held at ± 1°C and the gas-phase composition was held to k0.2 pet NH3. Based upon the results of numerous diffusion experiments with this alloy* the 'Results to be published in a third paper of this series. times chosen for equilibration were considered more than adequate, Nitrogen Isotope Exchange. The first exchange experiments were carried out by circulating a measured quantity of H2 and NH3* (with a predetermined isotopic *The NH3 was synthesized over a synthetic ammonia iron catalyst using H2, and N2, enriched with N15. AS the NH3 was formed it was removed continuously from the gas phase by circulating the mixture through a refrigerated (78ºK) trap. When most of the nitrogen had been converted to NH3, it was distilled from the trap into a glass storage vessel. composition, N15/N14) over a nitrided specimen at 450°C in a closed glass system. Attempts to reach the exchange limit isothermally, i.e., an isotopic ratio (N15/N14) in the gas phase identical with the extractable nitrogen in the nitrided alloy, were futile. The exchange rate between the gas phase and the alloy was too slow, involving many days. To circumvent the slow exchange with the gas phase, measured amounts of N15 and N14 were introduced into the alloy by nitrogenating with an NH3-H2, mixture at 500°C containing an N15/N14 ratio of 7.76; the charged specimens were then sealed by allowing an oxide film to form over them in air, and in this final condition the specimens were subjected to 500°C in vacuum for various times during which isotope exchange was allowed to proceed within the specimen. It was estab-

Jan 1, 1970