Search Documents

By B. N. Das, J. B. Darby, P. A. Beck, Y. Shimomura

A POWDER pattern for the (Cr, Mo, Co)R-phase annealed at 1200°C was reported in 1951.1 Through the courtesy of Prof. D. P. Shoemaker of Massachusetts Institute of Technology the authors became aware of inconsistencies of this pattern with that to be expected from the structure of the R-phase, as determined by Komura, Shoemaker, and Shoemaker.' In addition, Professor Shoemaker also noted that the powder pattern reported8 for the (Cr, Mo, Co)D-phase, annealed at 1300°C, agreed fairly well with that to be expected from the newly determined structure of the R-phase. In view of these findings, the previously reported powder patterns of the R-phase and of the D-phase were compared carefully. It was found that most lines in the two patterns (22 lines) were to a fair degree of accuracy related to each other by a single conversion ratio for the corresponding d spacings. The value of the conversion ratio was found to be 1.0058, so that the d spacings of the D-phase pattern previously reported were larger than the correspond- ing d spacings for the reported R-phase pattern by approximately that factor. The intensity relationships between corresponding lines in the two patterns were similar, as judged visually. The following exceptions were noted: Lines Nos. 2, 3, 19, 20, 21, 22, 23, 24 and 25 of the D-phase pattern,:' all designated weak or very weak, were missing in the apparently somewhat fainter R-phase pattern used.' Lines 1, 2, 3, 5, 15 and 34 (all weak or very weak), reported for the R-phase, were missing in the D-phase pattern, Table I. In view of these observations it seemed probable that the two patterns differed from each other mainly by a slight change in lattice parameters (with c/a remaining approximately constant), and that the pattern previously reported for the R-phase contained some weak extraneous lines, most likely to be attributed to impurities. In order to check the foregoing assumption, two specimens of an alloy containing 43 pct by weight of cobalt, 41 pct molybdenum, and 16 pct chromium, which was within the composition range of stability of both the D-phase at 1300°C and of the R-phase at 1200°C, were homogenized at 1200 and 1300°C, respectively, and quenched. X-ray diffraction patterns of the powders of these two specimens, obtained with CrK radiation, were compared carefully with each other and with the D-phase pattern previously

Jan 1, 1959

By R. J. Wasilewski

The resistivity of single crystal and of polycrystalline metal has been determined between 77° and 1500°K. At comparable purity, the resistivity of the poly crystalline metal differs from that calculated from the axial resistivity values. The observed anisotropy is briefly discussed. A zone refined titanium rod was obtained from F. J. Darnell.1 The hardness of this material varied between 52 and 64 Bhn, indicative of its high purity. Single-crystal specimens were cut out from a few large grains, elongated predominantly along <1120>. Resistance measurements were taken with specimens immersed in liquid nitrogen, solid CO,, and acetone, and at ice point, and then recorded continuously between room temperature and 1200" to 1250°C, throughout at least one full heating and cooling cycle at a rate of l° to 3°C per min. Four probe measurements were taken using spot-welded Pt wire 0.003 in. in diam as potential terminals, and the electromotive force drop was determined poten-tiometrically. A standard resistance, in series with the specimen, served to determine the dc current (generally about 80 ma) in the circuit. In order to eliminate spurious thermal electromotive forces, the circuit polarity was automatically reversed at 5-min intervals, and the mean of the two adjacent readings taken as the true electromotive force value. The discrepancy between the readings at reversed polarities was generally of the order of a few µ v, as all the spot-welded joints were contained within a volume of some 5 mm cube. The relative resistance (R T/R 273o) variation with temperature is tabulated below, and shown in Fig. 1, as measured during the first heating run. The discontinuous drop in resistance, corresponding to the a — ß transformation, started for both initial orientations at 1170°K; i.e., some 15°K above the accepted value of 882°C (1155°K). Judging by the temperature ranse of transformation—some 30°K for the single crystal and 20°K for the polycrystal-line specimen—this difference is believed caused by the solution of the oxygen present initially on the surface of the specimens. The general trend of the resistance vs temperature shown in Fi,;. 1 is in qualitative agreement with that previously reported for polycrystalline titanium metal. 2,3 Significant anisotropy is, however, indicated by the crossing over of the curves for <1120> and <0001> orientations at 273°, 650°, and 1000°K. This difference is most startlingly shown in Fig. 2, where instantaneous temperature coefficients (l/R273 x dR /dT) are plotted for both the first heat-

Jan 1, 1962

By Nathaniel Herz

(San Francisco Meeting, September, 1915) THE use of zinc dust for precipitating the precious metals from cyanide solutions is well established now in many places, and has many advantages over the shavings method of precipitation. Although much work has been clone on methods of testing zinc dust, as yet no absolutely positive test has been devised to determine the value of the material. Certain facts are known, but often it happens that results on a working scale are not as expected from the laboratory tests. The purpose of this paper is to record some observations made while testing. a large variety of zinc-dust samples in the laboratory. W. J. Sharwood1 has described standard analytical methods, which have been followed, with the changes noted. The regular determinations include zinc oxide, by solution in ammonia and ammonium chloride, lead, and precipitating efficiency. In some cases cadmium was determined by a method similar to that described by J. E. Clennell.2 I will discuss the precipitating-efficiency test in detail. The procedure is as follows: "A solution of potassium silver cyanide is prepared by dissolving 10 grams of silver cyanide (AgCN) and 5 grams of `99 0&apos; potassium cyanide in a little water and diluting up to 1000 cc. It is then adjusted by addition of a little more KCN or AgCN until the solution indicates from 0.12% to 0.15% free KCN by titration with standard silver nitrate. The titration is best made by using a 10-cc. or 20-cc. sample, adding 1 cc. of 2 % potassium iodide, and a slight excess of ammonia, as the end point is then sharper. Or 15 grains of pure crystallized KAg(CN)2 may he dissolved in a liter of water and 1.5 grams KCN added. "Weigh out 0.5 grain zinc dust into a 300-cc. beaker. Add a few cubic centimeters of water and stir until, zinc is well mixed, then pour in 250 cc. of the prepared solution, stirring vigorously. See that all lumps are broken up, and continue stirring for fully five minutes. Stir occasionally (at least every 10 minutes) until the end of two hours from the addition of the solution. Then filter upon an 11-cm. filter, wash precipitate thoroughly, sprinkle with test lead, wrap it carefully in the paper, plaice in a scorifier with about 20 grams test lead, burn paper cautiously in muffle, scorify five minutes, cupel at low temperature and weigh silver. Milligrams silver obtained from 0.5 gram zinc X 0.0606 = percentage precipitating efficiency."&apos;

Jan 8, 1915

By John B. Hastings

THE origin of the watery vapors of vulcanism has always been an object of interest and speculation to the seismologist, and as theories of the genetic origin of ore-deposits have of late years been pretty well narrowed down to the expiring forces of plutonic action, the same question has had a lively interest for mining engineers and geologists, as is well shown by the discussions of the subject in our Transactions. The important part taken by volcanic emanations in the origin of pegmatites and quartz-veins, described in my paper, Origin of Pegmatite,1 and their latent power to concentrate into useful deposits such scattered gold as occurs in the Hartsel granite, make a discussion of their derivation but a natural third and final step. It is conceded that enormous amounts of vapor accompany volcanism, though perhaps we are apt to forget that steam has 1,700 times the volume of water, besides which the column seen over Vesuvius and other volcanoes is greatly mixed with air; the immensity of such volumes compared with solids and liquids is shown by the experiment of Gautier, who, by heating dessicated granite to 100° C., evolved from it uses 20 times, and steam 90 times, its own volume. Dana appraised the average amount of water left in ordinary rocks as 2.5 per cent. T. M. Read estimated that the Mississippi river carries to the sea annually 150,000,000 tons of rock material. If these Mississippi sediments, as deposited, contained 20 per cent. of water, it would be 600,000,000 cu. ft., or 4,500,000,000 American gallons, annually. Allowing the vapor suspended over a volcanic cone to be mixed with 80 per cent. of air, this amount of water converted into steam would replenish anew, every 9 min., a column 15,000 ft. high, 2,000 ft. in diameter at the base, and 10,000 ft. at the top. Read&apos;s estimate is only half of the amount given in a more recent and probably correct one .2

Jan 5, 1908

By C. D. Tedmon, D. P. Ferriss

THE yield stress, o of low-carbon steel has been shown to vary with the average grain diameter, d, according to the relation1-3 where o is taken to be the lower yield-point stress Of is the friction stress on an unlocked dislocation, and ky is a constant. The interpretation2,4 of ky in terms of dislocation theory relates this constant to the stress to unlock a source across a grain boundary. cottrel14 predicted that ky would increase with decreasing temperature. This was observed to be the case by Adams and coworkers5 in their investigation of niobium (columbium). However, petch6 and Backofen: both working with low-carbon steel, found ky insensitive to temperature. In his work with high-purity niobium, Johnson&apos; found ky equal to zero. Evansg showed that k, was essentially zero for niobium containing nitrogen in an appreciable concentration range. The present experiments were designed to check this apparent anomaly in the value of ky in another Group V metal. Yield points were determined as a function of grain size at several temperatures for tantalum and a tantalum-tungsten alloy. The material used was double are-melted tantalum and a double are-melted alloy of 90 pct Ta and 10 pct tungsten (by weight), both obtained as unannealed, swaged rod. The impurity content of the materials is given in Table I. The tantalum was annealed at 1325"C. in a vacuum resistance furnace using a tantalum boat. The alloy was similarly annealed at 1660°C. Annealing times varied from 15 min to 2 hr, depending on the desired grain size. Nominal pressure in the furnace was 3 X 10~4 mm of Kg. Metallographic examination showed that the annealing treatment produced grain sizes ranging frorn 0.021 to 0.200 mm in the tantalum, and 0.060 to 0.160 mm in the alloy. Tensile bars were made by centerless grinding the annealed specimen;, and then electropolishing to remove all grinding marks. The specimens were than pulled :it 2 1/2 pct per rnin in an Instron testing machine. The tantalum specimens were tested at 77", 195", and 300°K. The alloy was tested at 300°K only. All specimens exhibited a yield-point phenomenon at all temperatures. Typical load-elongation curves at the three test temperatures are shown in Fig. 1. The lower yield stress is plotted as a function of (grain size) in Figs. 2 and 3 for tantalum and the 90 pct Ta-10 pct W alloy, respectfully. The position and slope of the curves was determined by least-

Jan 1, 1962

By A. Aly Selim

A computer model was developed to calculate the fragmentation cost for in situ leaching operations as a function of the blast design and deposit parameters. The model is based on blasting an ore zone only or an ore zone plus overburden by either a coyote blast or a vertical blasthole system. The model calculates the blast design parameters and the fragmentation cost based either on a user input powder factor value or on a powder factor calculated by the model as a function of the overburden height and the ore zone thickness. Examples of blast design parameters calculated by the model are the number and spacing of blastholes for a vertical blasthole system and the number and spacing of crosscuts for a coyote system. The model also calculates the total amount of explosives, the detonating cord length, and the number of primers. The cost of blasthole drilling can be calculated by the model based either on purchasing and operating a drill or on a user input value of the contracted cost of drilling. Application of the model to an example ore deposit showed that the vertical blasthole systems were more economical than the coyote system when there was no overburden and the deposit had an average ore thickness less than 45 meters. With no overburden and ore thickness greater than 45 meters, the vertical blasthole system was either more or less expensive than the coyote system depending on the number of levels used in the coyote system. With overburden, the coyote system was less expensive than the vertical blasthole system for blasting either the ore only or the ore plus the overburden. A coyote blast will usually produce larger particle sizes than a vertical blasthole system. Larger particle sizes can result in lower copper recoveries so that a less expensive coyote blast may not improve the overall economics of an in situ leaching operation. Blasting the ore zone only was generally less expensive than blasting the ore plus the overburden by either blasting system. Also, for the example considered, the coyote system costs were less sensitive to changes in overburden thickness and powder factor while the vertical blasthole system costs were less sensitive to changes in ore thickness.

Jan 1, 1977

By J. B. Darby

In an investigation of various equiatomic alloys of transition elements, Dwightl did not find evidence for the CsC1-type ordered structure in VMn. More recently waterstrat2 has reported the occurrence of this structure in the alloy his sample had been homogenized at 1150°C and subsequently reannealed at 725°C after crushing to powder. The purpose of this note is to confirm the existence of the CsC1-type ordered structure in VMn and to report a lattice parameter. An equiatomic alloy was prepared by arc-melting under an argon atmosphere vanadium and electrolytic manganese having a purity of at least 99.9 pet. The composition was obtained by charging an excess of manganese and monitoring the weight loss until the stoichiometric composition was achieved; the assumption that the loss during melting was due to the vaporization of manganese appears to be a valid one.&apos; The calculated composition of the sample prepared was 49.85 at. pct V and 50.15 at. pct Mn. Specimens taken from the fractured as-cast buttons were wrapped in molybdenum foil and encapsulated in quartz capsules under vacuum; there was no evidence of a reaction between the alloy and foil. The X-ray patterns were obtained using filtered copper or chromium radiation with a Straumanis-type Debye-Scherrer camera having a diameter of 114.6 mm. The CrKa radiation is best suited for detecting the superlattice lines since it overcomes the slight difference in scattering powers of the components by making use of the anomalies in atomic scattering factor which occur when the frequency of the radiation is close to the characteristic absorption frequency of one of the elements.394 A specimen in the as-cast condition, as well as one which had been annealed for 1 week at 900°C and water-quenched, gave a diffraction pattern for the disordered bcc solid solution. However, when samples were homogenized at 900°C for 3 weeks followed by a subsequent anneal at 700°C for 6 to 7 weeks and then water-quenched or furnace-cooled, the (loo), (1111, and (210) Ka superlattice lines were observed in films taken with chromium radiation. An ao = 2.904 * 0.001 was determined by a Nelson-Riley extrapolation from a film taken with CuKa radiation. The author wishes to thank Mr. J. W. Downey and Mr. L. J. Norton for carrying out the experimental portion of this investigation. This work was performed at the Argonne National Laboratory under the auspices of the U.S. Atomic Energy Commission.

Jan 1, 1963

By Charles Barrett

THE orientation of metal crystals and grains, both large and small,. can be determined conveniently and accurately without the use of X-ray apparatus. This seems to be appreciated by so few metallurgists that it may be useful to explain in detail the method we have found most satis-factory in the laboratory the reflection of light from crystallographic etch pits. This note includes a description of a suitable inexpensive instrument and instructions for etching various metals and for plotting the data. As the stereographic projection is used to facilitate handling the data, this note may be considered as an appendix to an earlier review of the metallurgical uses of the stereographic projection.1 Various methods involving etch pits have been used by other investi-gators, Bridgman&apos;s method2 consists of attaching the specimen to a sphere (a transparent sphere is convenient4), holding it at arm&apos;s length, and marking a spot on it when it has been turned so that the etch pits reflect light into the eye of the observer from a lamp standing behind him. It has an accuracy of about 2° and is extremely rapid. A greater accuracy can be obtained by having the reflected light fall on a screen, as has been done by Czoehralski, 5 Chalmers,6 and Schubnikov.7 All of these methods have been intended for undeformed single crystals. Tammann and his coworkers"&apos; developed a method for estimating the number of grains in a polycrystalline aggregate having orientations in a given region of the stereographic triangle and thus obtained statistical information about deformation and recrystallization textures. While the method has had some use in recent years,9 it is not applicable to the majority of problems in physical metallurgy. Smith and Mehl10 determined orientations by plotting the directions of the sides of individual etch pits on a stereo-

Jan 1, 1940

By E. Miller, J. M. Eldridge, K. L. Komarek

The liquidus curve of the Mg-Pb system was accurately redetermined. The compound Mg2Pb decomposes peritectically at 538.2° ± 0.3°C to liquid and to a compound p&apos; which melts congruently at 35.0 at. pct Pb and 549.0° ± 0.3°C. The solidus curve of ß&apos; was determined. X-ray diffraction studies indicate that 4&apos; has an orthorhombic structure. Activity values of magnesium calculated from the phase diagram agree with those published in the literature. EXPERIMENTAL thermodynamic properties of binary metallic systems have to be consistent with values calculated from the phase diagram. In systems forming intermetallic compounds the shape of the liquidus curve near a compound is determined by the thermodynamic properties of the coexisting solid and liquid phases. Hauffe and Wagner&apos; neglected the temperature dependence of the chemical potentials and obtained the potential differences of the components of the liquid alloys, relative to stoichiometric liquid. Their calculations were based on the liquidus curve and on the heat of fusion of the compound, and were only valid near the congruent melting point. Steiner, Miller, and Komarek2 developed equations which account for the temperature dependence and obtained the chemical potentials of liquid Mg-Sn alloys over the entire phase diagram from the liquidus and solidus curves and from enthalpy values with the pure components as the standard states. The Mg-Pb phase diagram has been studied by several investigators whose results have been compiled and critically evaluated by Hansen.3 Although the liquidus curve was poorly defined, the general features of the diagram, i.e., one congruent melting compound, Mg2Pb, of essentially stoichiometric composition, two eutectics, and limited terminal solid solubilities, seemed to be suitable for a similar thermodynamic analysis. A careful redeter-mination of the liquidus by thermal analysis revealed, however, the existence of another compound. The liquidus curve between the two eutectics was precisely delineated and the structure and solidus curve of the new compound were investigated. The revised phase diagram was thermodynamic ally analyzed to evaluate the activity of magnesium in the liquid alloys. EXPERIMENTAL PROCEDURE The magnesium metal (Dominion Magnesium Ltd., Toronto, Canada) had a purity of 99.99+ pct; lead (American Smelting and Refining Co.) contained 99.999 pct Pb. Most experiments were carried out in graphite crucibles. Several experiments were made in high-purity alumina (Triangle R.R., Mor-ganite, Inc.) and in Armco iron crucibles to test the inertness of the graphite crucibles. Chemical analysis of magnesium and detailed description of the procedure for thermal analysis have been given previously. For the determination of the solidus curve of the compounds, specimens of initial composition Mg2Pb were equilibrated in a closed isothermal system with magnesium vapor. The source of the magnesium vapor was an alloy which had a gross composition lying in the 0&apos; + L field at the temperature of equilibration. As equilibrium was approached, the specimens lost magnesium to the two-phase reservoir thereby lowering the activity of magnesium in the specimens until activity and composition equaled that of the ß&apos;/ß&apos; + L boundary. Crucibles (1.9 cm ID by 2.2 cm OD by 4.1 cm high) and tightly fitting lids were machined from a molybdenum rod; small, shallow trays were fashioned from thin (0.005 in.) molybdenum sheet, and all the molybdenum components were degreased in hot carbon tetrachloride and then dried. The pieces were then degassed in vacuum at 950°C for about 6 hr. The two-phase alloy was placed at the bottom of the crucible and small specimens of the Mg2Pb compound, weighed on an analytical balance, were placed in two molybdenum trays above the two-phase alloy. The crucible was closed by forcing its lid on and then inserted in a titanium crucible. This crucible was evacuated, flushed twice with argon, and welded under argon. The specimens were equilibrated for about 1 week in a resistance furnace regulated by a Celectray controller, and the runs were terminated by water quenching. The specimens were again weighed and the equilibrium compositions were calculated on the basis that the weight losses were solely due to a loss of magnesium to the two-phase alloy. The structure of the B&apos; phase was investigated by the Debye-Scherrer X-ray diffraction technique. Selected ingots from thermal-analysis experiments containing about 35 at. pct Pb were re-melted, slowly cooled, and crushed in an argon-filled glovebox until the entire ingot passed through a 50-mesh sieve. The powder was thoroughly

Jan 1, 1965

MRS. SIDNEY J. JENNINGS, President MRS. ARTHUR S. DWIGHT, First Vice-President MRS. KARL EILERS, Second Vice-President MRS. H. W. HARDINGE, Third Vice-President MRS. BRADLEY STOUGHTON, Recording Secretary MRS. AXEL 0. IHLSENG, Corresponding Secretary MRS. HARRIS K. MASTERS, Treasurer Welfare Committee MRS. C. C, BURGER, Chairman Sub-Committees Americanization Belgian Relief MRS. LEVI HOLBROOK, Chairman MRS. HENRY H. KNOX, Chairman Emergency MRS. HERMAN A. PROSSER, Chairman A very successful meeting Of the Council of the Woman&apos;s Auxiliary was held Wednesday, July 18, and plans for war relief work were thoroughly discussed. The Belgian Relief Committee has sent out the following letter to the ten local sub-committees, which were formed to raise money to feed the Belgian children: "The Commission for Relief in Belgium announced in a letter from Mr. Hoover that after the first of June the United States Government would take over the relief of Belgium and Northern France and called attention to the following paragraph: ?Naturally, having built up such an effective organization you will desire to keep it alive as far as possible, and we venture to suggest that, although the general relief of the countries involved will now be met by the Government appropriations, emer-gencies and special conditions may arise which could only be met by private donations. In such circumstances your organization will afford a ready means of meeting the demands of the situation, whatever they may be. Should any of your contributors

Jan 9, 1917

By P. R. Sperry, P. A. Beck, J. Towers

Dahl and Pawlek1 found that electrolytic copper develops extremely coarse grains at 1000°C after about 90 pct reduction by rolling. This coarsening occurs only under conditions of penultimate grain size, deformation, and alloying which lead to the "cube" recrystallization texture.l,2,3,5 The peculiar angular shapes and straight grain boundaries of the coarse grains were noted by several investigator.1,4,5 On the other hand, coarsening in Fe-containing aluminum or in AI-Mn alloys8 does not depend on a "cube" (or any well developed) recrystallization texture. It is true that increasing deformation by rolling, and, therefore, an increasingly well developed re-crystallization texture, are associated with decreasing incubation periods of coarsening.6-7-8 Nevertheless, coarsening readily develops in aluminum even after only 30 pct reduction by rolling, where the recrystallization texture is very weak.6,8 Also, coarsening was observed by Jeffries9 many years ago in sintered thoriated tungsten, which presumably has no preferred orientation. In all these cases coarsening is associated with grain growth inhibition by a dispersed second phase.8,9 The annealing temperature has to be suficiently high to overcome the inhibition at a few locations. But if it is too high, growth starts at many points, and the resulting grain size becomes much smaller.9 Normally, the coarse grains are more or less equiaxed, and the boundaries have a typical ragged appearance.6.8 Cook and Macquarie4 demonstrated that, in addition to the texture-dependent coarsening previously found at 1000°C,l electrolytic tough pitch copper may also coarsen at 800°C after 50 pct reduction by cross rolling. The coarse grains formed under such conditions have rounded shapes and ragged boundaries, like those in aluminum. When the annealing temperature is higher, the tendency for their formation decreases. All these observations suggest that the coarsening at 800°C is associated with inhibition by a second phase. Actually, coarsening at 800°C after 50 pct reduction by cross rolling was observed only in tough pitch copper,4 which contains Cu2O particles. On the other hand, the texture-dependent 1000°C coarsening occurs in both tough pitch and oxygen-free copper;4 it does not appear to depend on the presence of a dispersed second phase. However, the interpretation of the 800°C coarsening in Cu after 50 pct rolling as an inhibition-dependent process, similar to the coarsening in A1-Mn alloys, is somewhat weakened by the fact that this coarsening was reported4 to occur only after cross rolling, and not after straight rolling. It was, therefore, decided to re-examine this question. A 1 in. diam electrolytic tough pitch copper rod, No. 2 hard drawn, was annealed for 20 min at 700°C, rolled to 0.5 in., annealed 10 min at 700°C, and straight rolled to 0.064 in. It was then given a penultimate anneal of 20 min at 500°C and it was cut into four sections, which were given final reductions by straight rolling as follows: A 30 pct reduction of area B 50 pct reduction of area C 70 pct reduction of area D 90 pct reduction of area Specimens cut from the four sections were finally annealed at 800°C in an oxidizing atmosphere. Strip A remained fine grained up to 10 hr, but the specimen annealed 12 hr consisted of only 2 large grains. Strip B had a few scattered large (1/2 to 3/4 mm) grains after 1 min, although the balance of the specimen consisted of fine grains of about 0.02 mm. After 5 min there were several 10 to 15 mm grains present, and after 1 hr strip B was completely coarsened. The coarse grains had the same characteristics (see Fig 1) as those obtained by Cook and Macquarie at 800°C after cross rolling. Strip C had several grains of 0.05 to 1 mm after 1 min, but it was still largely fine grained after 12 hr. After 48 hr it consisted entirely of grains of about 0.5 to 4 mm, with an extraordinarily large number of twin bands. Strip D remained com- pletely fine grained after 4 hr at 800°C. These results indicate that, in the deformation range of 30 to 70 pct reduction, the incubation period for coarsening as well as the rate of growth and the final size of the coarse grains decreases with increasing deformation. Similar

Jan 1, 1950

By J. P. Morris

PREVIOUS investigations1,2 have shown that alloying elements in liquid iron influence the thermodynamic activity of sulphur and thereby affect the partition of sulphur between metal and slag in the desulphurization process. For example, the greater efficiency of desulphurization in the blast furnace as compared to the open hearth can be attributed in part to a higher level of sulphur activity in blast-furnace metal due to the higher concentration of carbon and silicon. In the present investigation, a short study was made of the influence of manganese on the activity of sulphur in liquid iron and iron-carbon alloys. In contrast to carbon and silicon, manganese was found to decrease the activity coefficient of sulphur; and in iron-carbon alloys it counteracts to some extent the influence of carbon. However, at manganese concentrations normally present in the blast furnace or open hearth, the effect of manganese is small. Since manganese sulphide has a limited solubility in iron, manganese can act, under certain conditions as a desulphurizing agent. Considerable data on the manganese-sulphur product in carbon-saturated melts were obtained in the investigation and have been included in this report. The experimental procedure was the same as that used in the earlier investigations on the effect of silicon&apos; and carbon&apos; on sulphur activity. Briefly, the method was as follows: The molten alloy, contained in a graphite or sintered alumina crucible, was brought to equilibrium at a constant temperature with a mixture of hydrogen and hydrogen sulphide of constant composition by bubbling the gas through the metal. Samples of&apos; the melt were taken for analysis at regular intervals by suction through a 2 to 3 mm bore silica tube dipped into the metal. The experiments were run in a graphite spiral resistance furnace with melts weighing 50 to 60 g. The gas bubbling tubes were made of sintered alumina and were 5/16 in. OD, 1/16 in. ID, and 24 in. long. Equilibrium was assumed to have been attained when the sulphur content of the liquid metal reached a constant value. During an experiment there was a rapid loss of manganese from the melt by volatilization. To offset this loss, small additions of manganese were made periodically. The rate of manganese addition needed to maintain a constant manganese concentration was determined in preliminary tests. In all of the experiments, deposits of manganese sulphide formed above the melts in a cooler region of the furnace. Apparently, these deposits resulted from a reaction between manganese vapor and hydrogen sulphide in the gas. To prove that manganese sulphide did not volatilize from the melts to a measurable extent, an experiment was run in which helium was bubbled through liquid iron containing both manganese and sulphur. Although manganese volatilized rapidly in this test, there was no appreciable loss of sulphur. Volatilization of manganese sulphide from a melt would have led to an apparent equilibrium condition in which the sulphur content of the metal was lower than the true equilibrium value. The experimental results are shown in the first seven columns of Table I. The data in the last two columns were obtained from the previous work on the effect of carbon&apos; and show what the results would have been in the absence of manganese but with temperature, gas composition, and carbon content of the metal remaining the same. Comparison of the last four columns show that, in the presence of manganese, the sulphur content of the metal increased at equilibrium and the activity coefficient of sulphur decreased. However, the results show that, for manganese concentrations below 3 pct, the effect of manganese is small. The values for activity coefficient of sulphur given in Table I were calculated from the following relations: S (in liquid metal) + H2 (gas) = H2S (gas) [l] K ph2s/?s X %S X phg = 0.00251 [2] where K is the equilibrium constant for the reaction, PH2S and ph2 are the partial pressures of hydrogen sulphide and hydrogen, respectively, and ?s is the activity coefficient of sulphur. The standard state for sulphur was taken to be a 1 pct solution of sulphur in pure iron. The numerical value for K at 1600°C was determined in the earlier work. For the purpose of showing graphically the results of the tests run at 1600°C, the activity coefficients of sulphur were recalculated so as to correspond to a manganese concentration in the metal of 2 pct in each case. In the calculation it was assumed that the increase in sulphur content of the metal at equilibrium caused by the presence of manganese

Jan 1, 1953

By William Wraith

1. INTRODUCTION. AT the Washoe smelter,. Anaconda, Mont., the blister-copper from the converters is transferred, by means of a crane, to a refining-furnace,, in which it is brought to proper pitch by means of air and poles. From this furnace the refined copper, containing gold and silver, is poured into cast-iron molds placed on a platform-conveyor, giving an anode 36.75 in. long, 28 in. wide, and 21 in. thick. By reason of a disagreement between the smelter and the refinery, in reference to the silver-content of the anodes, it became necessary to investigate the methods of sampling used. II. SMELTER METHOD OF SAMPLING. At the smelter the sampling is done by " spotting " into water a small portion of the molten stream of copper as it flows from the furnace, by batting" the stream with a wooden paddle. The first sample is taken 30, min. after the pouring is started, three. other samples being taken at 1-hr. intervals, each sample weighing from 4 to 6 oz. The samples are dried, examined for particle&apos;s of burnt wood, screened on a 10-mesh screen of No. 8 wire to remove the fines, the oversize then screened on a 4-mesh screen of No. 20 wire to remove the coarse, the undersize of this screen being taken as the sample. Teh four portions thus obtained are thoroughly mixed and spli in half by passing over a 16-slot splitting-device, slots being 0.5 in. wide. One-half of the sample is sent to the laboratory for analysis and one-half kept as a duplicate. III. REFINERY METHOD OF SAMPLING. The method used at the refinery and also used in this investigation is the one developed by Dr. Edward Seller, of

Mar 1, 1910

H. W. Turner, Portland, Ore. (communication to the Secretary*) :—Mr. Brown&apos;s paper on the complicated groups of veins exposed in the workings of the Bodie mine forme a valuable contribution to the literature of the structural features of ore-depoeits. It is much to be desired that managers should put into print the results of their observations of the mines under their charge. These observations, as well as data of production, kind of ores, etc., usually accumulate for years, and unless the mining geologists of the Geological Survey happen along before the mine is worked out, such data seldom get into print. About the year 1899 I went through the mines at Bodie with R. C. Turner, then superintendent, and made some notes on the veins and gangue-minerals, and collected some specimens. Mr. Brown refers to crystals of feldspar (albite) found on fragments of quartz on the surface. I collected a number of specimens of these crystals, mostly from Queen Bee hill, and

Jan 1, 1909

By John E. O’Rourke, Kevin M. O’Connor, Pamela H. Rey

INTRODUCTION The resurgence of coal mining activity in the United States, brought on by the spiraling costs of fossil fw1 energy in the Seventies, has come at a time of intense public concern for the quality of the environment. Notwithstanding pressure on our economy to develop alternate sources of fue1 energy to the import of oil, the legislatures of several states have reacted to public concern over the environment by passing strict regulations aimed at con- trolling the subsidence effect s of underground mining. Agencies of the federal government charged with assistance to the mining industry, including the Department of Energy and the Bureau of Mines, have sponsored a number of instrumentation and field measurement projects aimed at the development of subsidence prediction models that can aid the mine operator&apos;s task of subsidence control. There are good empirical models developed in Europe for subsidence prediction, but they were made possible by a large body of mining-induced subsidence data collected there over a long period of time. No com- parable subsidence data base exists in the United States, and consequently empirical modeling of subsidence is not a realistic approach for our near term needs. Moreover, the geologic and topographic diversity of the several coal regions in the United States is expected to necessitate the development of several empirical models, each one expected to be relevant to its own region. Because of the time and costs that are likely to be involved in an empirical modeling approach, it is considered more expedient and cost effective to develop a general, mechanistic model for subsidence prediction purposes. In order to develop such a model, it is necessary to investigate and quantify the mechanics of the subsidence process from the mine level up to the ground surface. The series of projects discussed in this paper are designed to achieve this objective and include the following work: (1) the identification of geotechnical instrumentation that will pro- vide mine level overburden and surface subsidence data. (2) a field demonstration of selected instruments, and (3) documentation of case histories for complete subsidence mechanics, using the demonstrated and preferred instruments. An identification of feasible instrumentation and monitoring techniques was completed by Woodward-Clyde Consultants (WCC) in 1977 (O&apos;Rourke and others). This paper discusses a demonstration of those instruments at a mine in Utah, and at two subsequent projects, currently underway at longwall mines in Colorado and West Virginia. &apos;he latter two projects when complete will provide documented case histories of subsidence mechanics. The process of optimizing subsidence instrumentation and monitoring techniques to the conditions encountered during installation and monitoring for these underground mines is shown to be an evolving one, and one which has had some notable successes to date. INITIAL DEMONSTRATION The initial design and demonstration of selected monitoring systems was carried out at the SUFCO No. 1 mine, near Salina, Utah. The instrumented panel was approximately 152 m wide. 640 m long. and was 290 m to 320 m deep. The mined height of coal. seam averaged 2.4 m. The mining method was room and pillar using continuous mining machines. This method allowed some monitoring of the supported condition during development, and eventually allowed monitoring of a caved system when both chain pillars and room pillars were extracted on retreat. The two instrument systems shown on Table 1 were selected from the earlier feasibility report for demonstration at SUFCO No. 1. Collectively, the two systems, one for a fully-supported mining method and the other for a fully-caved method, incorporate most of the instrumentation to be found within all five systems listed in the earlier feasibility report. The instrumentation includes surface, subsurface and mine monitoring installations. All of the SUFCO instruments selected to meet the specifications of the general instrument types listed on Table 1 were manually operated. That is, data from the installed system could only be obtained while a person was there to physically observe or operate the system readout. Automatic data recording equipment was available for some installations, but the objectives were to keep the systems as simple as possible for the demonstration project. A complete description of the surface, sub- surface and mine level instruments, and the demonstration project results are given in WCC (1982), and selected features are discussed in this paper.

Jan 1, 1982

By S. Chander, D. W. Fuerstenau

The inherently sluggish nature of the reactions involving sulfide minerals, particularly molybdenite, in aqueous solutions under ambient flotation conditions make their investigation complicated and difficult. Since the physicochemical nature of sulfides is known to be controlled by electrochemical reactions, a number of attempts have been made in the past to study sulfide mineral-collector interactions through rest potential and electrode polarization measurements. The purpose of the present investigation was to study the interaction of potassium diethyldithiophosphate (KDTP) with molybdenite. In the present investigation of the interaction of KDTP at the molydenite surface, molybdenite electrode rest potential measurements and electrode polarization behavior were experimentally determined under various solution conditions. The standard reduction potential for the equilibrium between dithiophosphate ions (DTP-) and bis(diethoxythiophosphoryl)disulfide (DTP) [(DTP). + 2e :i7-± 2DTP- (1)] can be evaluated from the electrode rest potential measurements on a platinum electrode in deoxygenated KDTP solutions saturated with freshly prepared (DTP)2. Experimental A platinum wire was used as the electrode for potential measurements. Prior to each measurement the elec-

Jan 1, 1975

Jan 1, 1964

By E. S. Machlin, W. R. Yankee

IN a previous study1 of the effect of heating com-mercial titanium in air on its subsequent friction coefficient against other metals, as well as itself, it was found that the friction coefficient markedly decreased from a value of about 0.7 to about 0.3. A tentative explanation was given that surfaces normally produced at room temperature are not contaminated sufficiently to prevent seizing or welding of the titanium to the softer mating metals. The latter tend to cleanse themselves during rubbing over the harder titanium. It was thought that the lack of a contaminant protective film on the titanium was due to the high solubility of titanium for oxygen and nitrogen and hence an inability to form a contaminant oxide or nitride. This explanation requires the ratio of the surface absorption rate to the diffusion rate to become much lower at room temperature than it is at high temperatures. In order to check the phenomenon further, commercial titanium specimens were nitrided or oxidized at 800°C for 20 hr in flows of prepurified N2 and 01, respectively, at about 1/2 in. H2O above atmospheric pressure. Friction runs were made in argon using a freshly cut copper hemisphere (cut in argon) on surfaces cut successively into the diffusion layers in the titanium (cut in argon) using the techniques described in a previous publication.&apos; DPH values (100 gram load) were made as a function of depth into the diffusion layer using a Tukon tester. Also, micrographs were taken at separate cross sections to indicate the diffusion layers. The results obtained are presented in Figs. 1 and 2, which show the "static" friction coefficient vs hardness for the nitrided and oxidized specimens, respectively. A separate measurement of the friction coefficient of clean copper vs iodide titanium also was made. From results reported in the literature&apos; giving the oxygen and nitrogen contents as functions of the hardness, cross plots were made showing the friction coefficients as functions of the amount of interstitial solute. These plots are given in Figs. 3 and 4. From micrographs of the diffusion layers and the phase diagrams, it was deduced that the data in Figs. l through 4 correspond to the single phase a region. The points observed on the compound regions have been excluded from the figures. It is apparent that nitrogen or oxygen in solution in the a titanium markedly affects the friction coefficient against a softer mating metal. Discussion of Results These results are extremely interesting from both a practical and theoretical viewpoint. The theoretical implications will be discussed first. According to Bowden, the friction coefficient should be given to a good approximation by the relation where a is the fraction of contact area that has welded, a is the shear strength of weaker component, and H is the hardness of softer component. Using this relation alone, it is difficult to understand the results because none of the terms should be affected by a variation in the oxygen or nitrogen content of the harder and stronger metal, titanium. Even if the ratio of S/H for titanium is used in Eq. 1, the ratio has been shown to be independent of oxy-gen or nitrogen content.&apos; If a more rigorous equa-tion is used combining Eq. 1 and a result given pre-viously" for the case where welding is absent, then the relation obtained is µ = a S/H + (1-a) a W aß/H where a is constant and Waß is the work of adhesion between the two metals comprising the friction couple. This relation states that if a is less than 1/2 or so, variation in the work of adhesion Waß between copper and the titanium should affect the friction coefficient markedly. It is reasonable to expect that the work of adhesion will depend on the oxygen or nitrogen content of the titanium. Available data4 show that clean metals and oxides have much lower works of adhesion than the same metals against the

Jan 1, 1955

Edwin H. MessiteR, New Pork City (communication to the Secretary*):—Under the heading " Flues," Mr. Edwards refers to the Bee-hive construction, a cross-section of which is shown in Fig. 4 of his paper. A flue similar to this was designed by me about six years ago,&apos; in which the walls though much thinner than those described by Mr. Edwards gave entire satisfaction. These walls, from 2.25 in. thick throughout in the smaller flues, to 3.25 in. in the larger, were built by plastering the cement mortar on expanded-metal lath without the use of any forms, or cribs, whatever, at a cost of labor generally less then $1 per sq. yd. of wall. Of course, where plasterers cannot be obtained on reasonable terms, the cement can be molded between wooden forms, though it is difficult to see how it can be done with an interior core only as stated by Mr. Edwards. In regard to the effect of sulphur dioxide and furnace-gases on the cement, I have found that, in certain cases, this is a matter which must be given very careful attention. Where there is sufficient heat to prevent the existence of condensed moisture inside of the flue, there is apparently no action whatever on the cement, but if the concrete is wet, it is rapidly affected by these gases. At points near the furnaces there is generally sufficient heat not only to prevent internal condensation of the aqueous vapor always present in the gases, but also to evaporate water from rain or snow falling on the outside of the flue. Further along, a point is reached where rain-water will percolate through minute cracks caused by expansion and contraction, and reach the interior, even though internal condensation does not occur there in dry weather. From this point to the end of the flue the roof must be coated on the outside with asphalt paint or other impervious material. In very long flues a point may be reached where moisture will condense on the inside of the malls in cold weather. From this point to

Jan 1, 1905

By M. Nicholas, D. M. Poole

The diameters of sessile drops have been found to increase linearly with time in five reacting binary metal systems. The spreading rates of the drops are markedly dependent on temperature and on prior alloying of the solid with the lower melting point metal, hut are independent of the drop volume, wetting atruosphere , solid-surface roughness, and prior alloying of the drop with the substrate metal. A mechanism has been suggested that relates the linear-spreading rate to lateral diffusion of the liquid-metal atoms into the solid at the drop edge. An Arrhenius- type equation has been derived that describes the temperature dependence 0) the spreading rate, and although the agreement between the actual and the predicted pre-exponen-tial terms is poor that between the activation energies is excellent and the variation in the spreading rate of copper on Ni-Cu alloys produced by different extents of alloying can be predicted with considerable accuracy. CHEMICAL interactions frequently change the wetting behavior of solid-liquid systems causing, for example, "secondary spreading1 of sessile drops beyond the size defined by the surface and interfacial tensions of the unreacted components. The kinetics of the contact-angle decreases associated with this spreading are similar for many systems, but few studies have been made with the objective of determining whether the similarities are a reflection of a common mechanism. Some workers2,3 have assumed the secondary spreading is controlled by changes in the liquid surface and liquid-solid interfacial tensions and hence by the composition of the liquid, and contact-angle changes measured by the vertical-plate technique have been used to follow the course of liquid-solid chemical reactions.4 Other processes that have been invoked to explain these time-dependent changes in specific systems include the removal of adsorbed gas from the liquid-solid interface.5 penetration of containment layers on the solid Surface,6 interdiffusion,1,7 reori-entation of the solid surface into a wettable configuration: vapor-phase transport of the liquid onto the solid in advance of the drop,9 and, from vertical-plate studies. capillary flow between oxide layers and the solid surface.10 One of the reasons for the profuseness of these suggestions may be the complexity of the contact-angle change kinetics. However, in an analysis of secondary spreading gold and copper on UC,11 it was found that the diameter of the contact area between the sessile drop and the solid surface showed a simple linear increase with time although contact-angle changes were more complex. To check whether the linearity was merely fortuitous! additional exploratory work was conducted with four reacting metal-metal systems: Au on Ni. Cu on Ni, Cu on Fe, and Ag on Au. Linear spreading was observed in every case even though the kinetics of the contact-angle changes were complex. A further detailed study of the kinetics of linear spreading of five reacting metal-metal systems has been made with the object of determining the mechanism involved. The influence of variables such as temperature, drop volume. and the initial composition of the drop on the linear-spreading rate has been measured and compared with those predicted by a number of possible mechanisms. The systems employed in this study (Cu and Au on Ni and Pt, and Ag on Au) were selected because of the availability of potentially relevant chemical and physical property data. the simplicity of their phase diagrams at the wetting temperatures, and the ease of experimentation. EXPERIMENTAL TECHNIQUES The purities of the metals used in the study were: copper, 99.9 pct; gold. 99.96 pct; nickel, 99.2 pct; platinum 99.99 pct; and silver, 99.999 pct. The wetting tests were performed in a split tantalum tube vacuum resistance furnace of a conventional design. The furnace element was held vertically and was 1 $ in. in diam and 6 in, long. Viewing ports were provided in the water-cooled chamber to enable the specimens to be observed in both the horizontal and vertical planes. The temperature in the hot zone of the furnace could be held at 1500" i 5°C for an indefinite time. The surfaces of the solid-plaque metals were ground flat on Microcut paper and both the sessile drop and substrate metals were ultrasonically cleaned in methyl alcohol prior to their insertion in the furnace. After loading, the furnace was pumped down to a pressure of 2 x 10-5 mm of mercury and degassed for 30 min at 900° to 950°C. The temperature was then increased at more than 100°C per min to that used in the wetting test. The vacuum at the wetting temperature was better than 5 x 10-5 mm of mercury. Dewetting and retraction of the drop on cooling did not occur and the contact-area diameters, therefore, were measured after solidification with a vernier traveling microscope. The diameters quoted later are arithmetic means of ten measurements. The standard error of the mean never exceeded 3 pct and was often less than 1 pct.

Jan 1, 1967