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By Milton Williams

It is generally recognized that fluid is lost from rotary drilling muds to permeable strata during normal drilling operations;1,2-3 but that this fluid is the filtrate from the mud, rather than the mud itself, has been shown by various workers.1,4,5 The presence of this filtrate in oil-bearing or gas-bearing strata is undesirable and harmful. The decreased permeability of the stratum to oil effected by the presence of water has been pointed out by several investigators,6,7 and since, in the production of the reservoir fluid, the greatest pressure drop occurs immediately adjacent to the borehole, it follows that infiltered water is particularly objectionable in this region. Again, this filtrate tends to make electrical logs less reliable, since oil in the proximity of the borehole is probably flushed out to an appreciable extent by the water.8 Observation of side wall cores may be misleading for the same reason. Drill-stem tests in low-pressure areas may be of doubtful value where no oil is recovered, unless sufficient time is allowed for production of water lost from the mud. The infiltered water may hinder drilling operations by softening shales and causing sloughing; the ['tight hole" occasioned by excessive deposition of filter cake in the hole is a common occurrence. The filter cake remaining on the face of the producing formation may itself sometimes be detrimental to production.9 In view of these implications of the importance of filtration of mud, an investigation was undertaken to determine the factors involved in the infiltration process, and to correlate these in such a manner that the values obtained in routine filter tests employing a conventional filter of the "wall-building tester" type,10 together with data on size of hole, drill pipe, and rate of mud circulation, could be used to estimate water loss and distance of penetration of the filtrate into strata. Quantitative relations of filter-cake permeability, filtrate viscosity, and rate of filtration have been developed for filtration in the simple laboratory filter.4a,11,12,13 It is obvious, however, that the conditions

Jan 1, 1940

By E. P. Pfleider, D. H. Yardley

Layers of magnetic taconite of above average magnetic iron content extend down dip on the Mesabi Range to depths beyond the reach of open pit mining. A selected layer with thickness of 75 to 100 ft underlies many square miles. Such a selected layer can provide over 50 million tons of recoverable concentratc per square mile, at lower concentration ratios than in the present open pit taconite operations. The system contemplated would consist of large scale underground quarrying by a lane and pillar method. Working heights would be 60 to 100 ft; room widths, 50 to 75 ft; and productivity targets, about 40 tons per man-shift. The most critical problems would he roof control and blasthole drilling. The successful operation of large open pits and concentrating plants for treatment of magnetic taconites indicates that the basic techniques and economic problems of pellet production have been solved. The open pit reserves are large, but they are not necessarily available in sufficient quantity or quality to provide an adequate raw materials base for all potential producers. Furthermore, as the more easily available open pit crudes are used up, the pits will become deeper, stripping costs per ton of concentrate will increase, and recoveries will decrease as leaner crudes are utilized. The time will come when supplementary and replacement reserves of magnetic taconite will be required. One way these can be obtained is by underground mining of the down-dip extension of the Mesabi magnetic taconites, especially those layers averaging well over 25% recoverable iron. A key point in such a proposal is the possibility of realizing substantial savings by beneficiating an ore of 30% magnetic iron at 2.5 to 1 ratio of concentration. This contrasts with current practice in Mesabi commercial taconite plants, where the ore averages 22 to 25% magnetic Fe, with concentration ratios of about 3.0 when producing 61% Fe pellets. Two factors which favor the eventual development of underground taconite mining are: 1) the desirable physical structure and high grade of taconite pellets in general and 2) the improved engineering techniques in underground mining. Experience in large scale room and pillar mines demonstrates that, given strong rock strata immediately above a high grade mining

Jan 1, 1963

By D. Cubicciotti

IT has long been known that some metals are capable of being dispersed or dissolved in certain of their fused salts.' Davy' and Bunsen³ were among the first to observe that in some fused salt electrolyses, a highly colored, strongly reducing salt phase appeared in the neighborhood of the cathode. Later workers found that the current efficiency of the electrolysis was markedly reduced when such a phase appeared. It was also found that the strongly reducing salt could be made by melting the metal and normal salt together. Chemical analysis showed that in such salts the metal ion to anion ratio was always larger than in the normal salt. From such observations arose two different explanations of the nature of metal in salt solutions. When a solution of this type is quenched, it is possible to find small globules of metal in the salt. From this and other observations, Lorenz' and co-workers assumed the metal in salt solution to be a colloidal dispersion of metal in the fused salt and called it "metallnebel" or metal fog formation. They made a number of experiments to substantiate this point of view. Another school felt that when the metal dissolved it reduced the salt partially to a mixture or solution of normal salt and subsalt. Both of these ideas could explain the strong reducing character of the salt formed and the low current efficiency of the electrolysis. If either a metal colloid or a subsalt were formed at the cathode and diffused to the anode, it would be oxidized to the normal salt. Thus a cyclic process of oxidation and reduction could be set up conducting the current without giving rise to a net change in the system. These facts led the author to investigate some of the properties of metal in salt solutions with the hope of elucidating their nature further. Among the metal-salt systems that form metal in salt solutions most markedly are the alkaline earth metal-halide systems and cerium, bismuth, and cadmium halides. Other systems of halides, oxides and sulphides form such solutions to a lesser degree. The first work undertaken was a study of the temperature-composition diagrams of some of the systems." From such diagrams it would be possible to distinguish between a subhalide formation or a colloid. A subhalide should give rise to characteristic changes in the phase diagram, while a colloidal dispersion of metal in salt would not alter the freezing point of the salt. The results obtained on a number of alkaline earth metal-halide systems were all quite similar. Fig. 1 shows the barium-barium chloride system. The other

Jan 1, 1954

By William Mikulas Lars Thomassen, Clair Upthegrove

Little work has been done in the field of the nickel-tin binary system. The complete diagram has been investigated on two occasions, but the results are in very poor agreement. The structure of a compound NiSn and the solubility of tin in nickel have been determined by X-ray methods. Several investigations have been made of the liquidus curve, and the compositions of the eutectics have been determined. A study of the literature, however, shows that there is no satisfactory agreement between the data presented in the various papers. The present investigation was undertaken in an attempt to determine the equilibrium conditions, and to correlate X-ray with metallographic data. The equilibrium diagram was determined by thermal and metallographic means, and the solubility of tin in nickel further investigated with X-rays. Powder diagrams were made of the intermetallic compounds, and three of the structures were partly determined. NO attempt was made to determine the range of homogeneity of the intermetallic compounds. Review of the Literature Vigorouxl prepared alloys of tin and nickel containing 74 and 92 per cent of tin. By treating these alloys with very dilute nitric acid or with sodium hydroxide he was able to separate residues, both of which analyzed 66.7 per cent tin. This corresponds to the compound NiSn and was reported as such. Guillet2 made the first investigation of the complete binary diagram Fig 1) The maximum point of the liquidus is at 43.5 per cent nickel. Several solid solution areas were found, and the compound NiSn was included on the strength of Vigoroux's work. The investigation was

Jan 1, 1937

By D. A. Bailey, F. L. Kadey

During recent years, expanded perlite has found extensive use in a wide variety of commercial applications. Specifications for a range of uses call for aggregates having different physical properties and requiring various types of processing. The mitre scopic examination of expanded aggregates in specially prepared thin sections has yielded important information regarding internal structure and can be a useful aid in evaluation of the product. Perlite is an acid volcanic glass containing from 2 to 5 pct combined water. When crushed and rapidly raised to a temperature of 1500° to 2100°F, the volatilization of the combined water, coincident with softening of the siliceous glass, causes the particles to expand or pop. Expansion of perlite to densities as low as 1-1/2 lb per cu ft has been achieved, although the normal range is from about 2.5 to 10 lb per cu ft. Low-density materials of this nature have found application in cryogenic insula- tions, insulating tile and board, plaster and lightweight concrete, soil conditioners, filter aids after comminution, and a host of other uses. The expansion of perlite may be controlled by a number of variables. Some of these are ore milling, furnace design, expanding temperature, use of preheating techniques, screen size distribution, and feed rate of the crude. For the specific intended uses, the art of perlite expanding has developed to the point that much is known about the effect of these variables on the end product. The requirements, however, for an aggregate to be used in plaster are different from those for an expanded perlite to be used in lightweight concrete or for cryogenics. In the study of perlite, many practical questions remain unanswered. One of the most important is, "why do some perlites make hard aggregates while others cannot resist crushing or compaction?" The usual tests and methods for evaluation of nonmetallic substances have been tried and have contributed their share to our knowledge. But chemical analyses, compaction resistance tests, screen analysis, etc., will reveal only a limited amount of information. The answers to these complex questions may well be found in an examination of the intemal structure of the expanded particle. Such questions and the ex-

Jan 1, 1962

By M. E. Shank, J. Wulff

In view of the current interest in magnetic materials having rectangular hysteresis loops, as for example those obtained with the grain oriented 50 nickel 50 iron alloys,t we wish to call attention again to the results obtainable with the perminvar (Co-Ni-Fe) alloys heat treated in a magnetic field. Data taken from direct current measurements made prior to and during World War II give the typical values shown below for two of the perrninvar alloys. Fig 1 and 2 show- the hysteresis loops for these samples. The first sample above consisted of small rings punched from 0.014 in. sheet stock. These rings were heat treated at 1000°C for one hour in a hydrogen atmosphere and then cooled with the furnace to 750°C at which point they were subjected to a magnetic field of 15 oersteds maintained during cooling to room telmperature. The molybdenum perminvar sample consisted of a spirally wound core of 0.001 in. tape. The heat treatment was the same except that box annealing methods were used and no hydrogen atmosphere was employed. Even better properties might be expected using hydrogen. The heat treating temperatures and cooling rates are not critical. Rectangular hysteresis loops produced in other perminvar alloys by heat treatment in a magnetic field were described earlier.',? Properties similar to those described above are realized in perminvars manufactured by conventional methods. Drastic cold working which in practice limits the final thickness and is gen- erally expensive may thus be avoided. This information may be of interest to those concerned with magnetic alloys and the development of contact rectifiers, magnetic amplifiers and so on.

Jan 1, 1950

By E. T. Turkdogan, Klaus Schwerdtfeger, P. Grieveson

The rate of growth of "Fe4N" on a iron was measured by nitriding purified iron strips in flowing am -monia -hydrogen gas mixtures at 504" and 554°C. It is shown that a dense nitride layer is formed when a zone -refined iron is used in the experiments. With less pure iron, the nitride layer is found to be porous. Through theoretical treatment, the self-diffusivity of nitrogen is evaluated porn the parabolic rate constant, and found to be essentially independent of nitrogen actirlity, e.g., D* = 3.2 x l0-12 and 7.9x l0-12 sq cm per sec at 504" and 554?C. Some consideration is given to the mechanism of diffusion in the nitride phase. THERE is a great deal of background knowledge on the solubility and diffusivity of nitrogen in iron, and on the thermodynamics and crystallography of several phases in the Fe-N system. Although case-nitrided steels have many applications in practice, no work seems to have been done on the diffusivity of nitrogen in the iron nitride, ?', phase. The only work reported on the related subject of which the authors are aware is an investigation by Prenosil,1 who measured the growth rate of the e phase on iron by nitriding in ammonia-hydrogen gas mixtures. EXPERIMENTS Purified iron plates of approximate dimensions 1 by 0.5 by 0.03 cm were nitrided in flowing mixtures of ammonia and hydrogen, in a vertical furnace fitted with a gas-tight recrystallized alumina tube. After a specified time of reaction, the sample was cooled to room temperature by withdrawal to the water cooled top of the reaction tube. The furnace temperature was controlled electronically in the usual manner within *l°C; the temperature was measured using a calibrated Pt/Pt-10 pct Rh thermocouple. For each experiment the iron strip sample was cleaned with fine emery cloth and degreased with tri-chloroethylene prior to the experiment. The ammonia-hydrogen gas mixtures were prepared from anhydrous ammonia and purified hydrogen using constant pressure-head capillary flowmeters. The gas mixture flowed upward in the furnace with flow rate of 400 cc per min at stp. The composition of the gas mixture was checked by chemical analysis at regular intervals. In most cases, the compositions of the exit gas and metered input gas agreed within about 0.3 pct, indicating that cracking of ammonia did not pose a problem at the temperatures employed. Two series of experiments were carried out using two different types of purified iron samples. In the first series of experiments at 550°C, vacuum carbon deoxidized "Plastiron" was used. The main impurities present in this iron were, in ppm: 4043, 50-Cr, 20-Zr, 40-Mn, 20-P, 20-S, 20-C, 50-0, and 10-N. In these experiments the rate data were obtained by measuring the change in weight of the iron specimen suspended in the hot zone of the furnace by a platinum wire from a silica spring balance. The nitride layer formed in these experiments was found to be porous, particularly near the outer surface. In other experiments, high purity zone-refined iron (prepared in this laboratory) was used. The total impurity content of this iron was 30 ppm of which 20 ppm was Co + Ni, 4 ppm 0, other metallic impurities were less than 1 ppm. The zone-refined iron bar, -2.5 cm diam, was cold rolled to a thickness of about 0.03 cm and the specimens were prepared for the experiment as described earlier. After the nitriding experiment, the sample was copper plated electro-lytically and mounted in plastic for metallographic polishing. After polishing, the thickness of the ?' layer was measured using a metallographic microscope. The nitride layer formed on the zone-refined iron was essentially free of pores. RESULTS The different morphology of the nitride layers grown on "Plastiron" and zone-refined iron is shown in Fig. 1. Both samples were nitrided side by side for 55 hr. The holes in the less pure iron, Fig. l(a), are confined to a region about one half thickness from the outer surface. The dense layer grown on zone-refined iron, Fig. l(b), is thinner than the porous layer on the "Plastiron". The impurities in the iron are believed to be responsible for the formation of a porous nitride layer. The pore formation may be due to the high nitrogen pressures existing within the nitride layer, e.g., the equilibrium nitrogen pressure is 1.2 x l05 atm in the 38.6 pct NH3-61.4 pct H2 and 6.6 x l03 atm at the Fe-Fe4N interface at 554°C and 0.96 atm. It is possible that the oxide inclusions present in the electrolytic iron may facilitate the nuclea-tion of nitrogen gas bubbles within the nitride layer. Support for this reasoning is the fact that pores are only encountered in the outer range of the layer where nitrogen pressures are largest. The photomicrographs in Fig. 2 show the effect of reaction time on the thickness of the dense nitride layer formed on zone-refined iron. These sections are from samples nitrided in a stream of 29 pct NH3-71 pct H2 mixture at 554°C for 22, 70, and 255 hr. In all the sections examined the nitride-iron interface was noted to be rugged. These irregularities are be-

Jan 1, 1970

By E. C. Robertson

Observations of faults in mines, at outcrops, and in the laboratory lead to the conclusion that the displacement d of a fault increases irregularly but monotonically with the thickness t of its associated fault gouge and breccia, not including adjacent undisplaced jointed rock. The general trend of data points has a slope d/t of about 100. (The correlation coefficient of a logarithmic regression line is r = 0.94.) The rather wide scatter of the points can be accounted for by inaccuracies in measurement of d and t, and by variation in the conditions at faulting of confining pressure, rock type, water pressure, and deformation history. Limestone is an exception to the relation. Until the data can be corrected and refined, the relation should be used only qualitatively for estimating displacement of ore bodies in mines. The suggested relation is based on observations of 48 steeply- dipping normal and reverse faults and nine small flat-dipping thrust faults, with displacement less than 5 km (3 miles). It does not apply to large strike-slip and low-angle overthrust faults because their large displacements are poorly determined and their breccia thicknesses are widely variable.

Jan 1, 1984

By D. W. Fuerstenau

MEASUREMENT of zeta potentials is a useful tool to study the surface chemistry of minerals under flotation conditions.1,2 Because there is continued interest in this approach, the apparatus for obtaining zeta potentials of nonconducting solids by the streaming potential method is outlined here. Fig. 1 illustrates the streaming potential apparatus." The streaming potential cell or plug consists of two 24/40 standard ground joints (4) joined with a piece of pyrex tubing 60 mm long and 12 mm in diam (5). The electrodes are made of bright platinum disks 19 mm in diam and 1 mm thick through which 0.5-mm holes have been drilled (6). To the surface of each is welded a piece of 80-mesh platinum gauze. Each electrode is permanently mounted on the ends of the inner parts of the two standard joints by means of a platinum wire (7) which connects it to the tungsten seal at the end of the cell (8). For ease in cleaning and handling the apparatus, the streaming cell is fastened to the 500-ml reservoir flasks (1) by means of two 18/9 ball and socket joints (2). This particular arrangement permits passage of the solution in either direction through the plug of particles. Flow of solution can be stopped by a stopcock (3). One of the reservoir flasks has a large opening to permit insertion of either a thermometer or a pair of electrodes for measuring pH of solutions within the system. In making the experiments, the plug is filled with 48 to 65-mesh particles, but a layer of 28 to 35-mesh particles is placed at each electrode to prevent any of the finer particles from passing through holes in the electrodes. The assembled apparatus is shown schematically in Fig. 2. To eliminate CO2 from the solutions, all experiments are conducted in a nitrogen atmosphere. Nitrogen, used to drive solutions through the plug, is passed through a bottle of concentrated KOH solution to remove CO2 (9). A 9-liter ballast reservoir (10) is used to maintain a more nearly uniform pressure. A series of stopcocks controls the direction of flow nitrogen to the flasks (11). Tubes of as-carite prevent backflow of CO2 into the system (12). Driving pressure, which can be set at any desired value, is measured with either a water manometer (13) or a mercury manometer (14). Reservoir flasks have side arms for making pressure corrections for the difference in water levels in the flasks. Streaming potentials are measured by the circuit illustrated in Fig. 2. The electrodes from the plug are connected through mercury wells (15) to a reversing switch (16), which reverses the polarity of the electrodes depending on the direction of flow of solution through the plug. The streaming potential is measured with a Leeds and Northrup type K2 potentiometer (17). Proper choice of null instrument is important because Eq. 1 assumes that the current which escapes through the measuring instruments is negligible. An ordinary galvanometer cannot be used to determine the null point because

Jan 1, 1957

By Henry J. Sandri

The use of economic models for forecasting purposes is an inexact yet necessary tool for mineral decision making. One method not commonly used is cyclical analysis because of its "non-scientific approach". However, under certain circumstances a modified cyclical approach can provide useful insight to mining companies. The current paper discusses mineral modeling, the type of economic models and the use of cyclical forecasting for mining firms (not speculators) involved in precious metals.

Jan 1, 1984

By F. G. Jones, R. D. Pehlke, H. E. Gardner

The solubility of nitrogen in liquid Fe-18 pct Cr-8 pct Ni-0. 7 to 2.3 pct A1 alloys has been measured up to the solubility limit for the formation of aluminum nitride in the temperature range 1600° to 1700°C uszng the Sieverts' method. The solubility of nitrogen in 18-8 stainless steel increases with increasing aluminum content. Based on a nitride composition, AlN, the standard free energy of formation of aluminum nitride from the elements dissolved in liquid 18-8 stainless-steel alloys has been determined to be: ?G° = -42,500 + 20. IT in the range from 1600° to 1700° C. EVANS and pehlke1 have measured the equilibrium conditions for the formation of aluminum nitride, AlN, in liquid Fe-A1 alloys. The present study extends that work to the more complex solvent, liquid 18 pct Cr-8 pct Ni (18-8) stainless steel. Recent work by Small and pehlke2 has dealt with the effect of fourth-element additions on the solubility of nitrogen in 18-8 base alloys. They found the effect of aluminum additions, up to 0.74 pct, on the solubility of nitrogen to be small. The present study covered the range from 0.74 to 2.28 pct aluminum, and by extending the composition range may be used to better define the effect of aluminum on the nitrogen solubility in these alloys. EXPERIMENTAL PROCEDURE The Sieverts' method was used to measure the equilibrium solubility of nitrogen gas in liquid 18-8 stainless steel alloys containing 0.74, 1.49, 1.93, and 2.28 pct Al. The solubility was measured as a function of the nitrogen gas pressure at temperatures of 1600°, 1650°, and 1700°C. The apparatus used is the same as described by Small and Pehlke.2 The 100-g melts were made from Ferrovac-E high-purity iron, Crucible Steel Co.; 99.95 pct Cr, Union Carbide Corp.; 99.9 pct Ni, International Nickel Co.; and 99.99+ pct Al, Aluminum Co. of America. The aluminum was charged at the bottom of the crucible, surrounded by nickel and iron. The chromium was packed into the interstices to minimize vapor transport of the aluminum during initial melting. The hot volume of the system, measured for each melt with argon, ranged from 45 to 55 standard cu cm with a temperature coefficient of —8 x 10-3 cu cm per °C. The melt temperature was measured with a Leeds and Northrup disappearing-filament type optical pyrometer sighted vertically downward on the center of the melt surface. The temperature calibration of the system by Small and pehlke2 was assumed. Two problems are involved in determining the solubility product of a solid, metal nitride phase in liquid iron alloys. These are: 1) establishing the point of departure from Henrian behavior at the solubility limit of the metal nitride phase; and 2) determining the composition of the solid nitride which is precipitated. Determination of the solubility product of AlN was made by admitting small amounts of nitrogen into the reaction bulb until the deviation from Sieverts' law was clearly evident in the form of a pressure halt. To obtain the solubility product at several temperatures during one run the following procedure was used: 1) add increments of nitrogen to determine the Sieverts' law line at the lowest desired temperature; 2) continue to add nitrogen to precipitate a small amount of the nitride phase; 3) increase the melt temperature 50°C to dissolve the precipitated nitride; 4) repeat step 2 until either a nitride formed or the system reached ambient pressure; if a nitride formed at 1650°C, the sequence was repeated at 1700°C. The composition of the precipitated phase was checked by an X-ray diffraction pattern obtained from powder scraped from the surface of the solidified 1.93 pct A1 melt. RESULTS AND DISCUSSlON Solubility Measurements. Fig. 1 is a typical nitrogen-absorption curve obtained from measurements on a 1.93 pct A1 alloy. Since the initial absorption of nitrogen follows Sieverts' law the nitrogen solubility is plotted as a function of the square root of the pressure of nitrogen gas in the reaction bulb. The results of the solubility measurements for all alloys studied are summarized in Table I. The slope of the Sieverts' law line for each alloy was determined. Since this is also the solubility of nitrogen at 1 atm pressure of nitrogen gas, the latter designation is used for the data. It should be noted. however, that in most cases the value lies above the solubility limit for AlN. Fig. 2 shows the effect of aluminum on the solubility of nitrogen at this reference pressure and as a function of melt temperature. The solid portions of the lines represent attainable solutions; the dashed regions lie above the limit for precipitation of AlN.

Jan 1, 1969

By W. I. Duvall

A brief review of the resonant frequency and ultrasonic pulse methods for obtaining elastic constants of rock samples shows that the equations for an iso-tropic elastic solid commonly used to calculate Young's modulus, modulus of rigidity and Poisson's ratio can result in appreciable error if the rock is even slightly anisotropic. Consideration of the equations that relate bar velocities and free medium velocities to elastic constants for orthotropic, transversely isotropic and isotropic solids shows that a combination of the two methods can be used to determine average elastic constants for a single sample of rock. The determination of elastic constants in different directions requires a large number of tests on oriented samples. The use of both the resonant frequency and ultrasonic pulse methods is recommended so that the determination of both Young's modulus and modulus of rigidity is independent of the determination of Poisson's ratio. The dynamic elastic constants of rock can be determined in the laboratory from measurements on small samples which may be in the form of right circular cylinders (diamond drill core). Either the resonant frequency6 or ultrasonic pulse method1 can be used to determine the longitudinal and shear velocities in the same specimen. The resonant frequency method provides a measure of the longitudinal bar velocity, V,, and the torsional bar velocity Vt; whereas the ultrasonic pulse method provides a measure of the free medium longitudinal velocity, Vp, and the free medium shear velocity, V, . The elastic constants (Young's modulus E, modulus of rigidity G, and Poisson's ratio v) are calculated from the density of the specimen, p, and one of the pairs of velocities by means of equations from isotropic elastic theory. For the resonant frequency method the equations are: It should be noted that Eq. 5 is derived from Eq. 4 and 6 and the relation between the elastic constants for an isotropic solid as given by the first part of Eq. 3. The in situ determination of dynamic elastic constants is accomplished by generating a complex seismic pulse in the rock and measuring the arrival times for the longitudinal and shear phases of the pulse at two distant points.5 From these travel times and the distance of the travel path both Vp and Vs are determined. The density of the rock is determined from samples in the laboratory, and Eq. 4 to 6 are used to calculate the elastic constants. These three methods involve the assumption of isotropy and perfect elasticity, and require the use of the relation v = (E/2G) - 1, which holds only if the elastic constants are the same in at least two directions. The calculation of v by means of Eq. 3 introduces considerable error, as a 1% error in V, and V, results in a 20% error in v. If frequencies for samples with a length-to-diameter ratio greater than four and a length greater than 8 in. are measured carefully, the experimental error can be kept to 1%. However, it is not unreasonable to expect that the variation in Vb and Vt with direction may exceed 1%. Thus, for even a small percentage of anisotropy the use of Eq. 3 can result in considerable error in v. The calculation of v by Eq. 5 also involves some uncertainty as a 1% error in Vs and Vp can result in a 6% error in v. By means of the pulse method both

Jan 1, 1965

By K. P. Gupta, A. K. Pal, L. Chandrasekaran, U. P. Singh

The Mn-Sn binary system, investigated at the high-manganese end and between 500° and 1000° C, shows four phases at temperatures below 727"C, namely the u Mn, the p Mn, the Mn3 Sn, and the Mn, Sn phases, while at higher temperatures only the last three phases remain stable. The solubility of tin in a Mn is very small and the maximum solubility of tin in P Mn phase appears to be abollt 10 at. pct Sn. The solubility range of the Mn,Sn and the Mn, Sn phases is 23.0 to 26.0 and 37.0 to 40.0 at. pct Sn, respectively. The lattice parameter of the 13 Mn phase increases with increasing tin content. The Mn, Sn thase is hexagonal with and appears to be basically of the Ni3 Sn type structure except that for quite a few X-ray diffraction lines the calculated and observed relative intensities do not agree well. The Mn-Sn binary system has been studied by several investigators.''~ Their results indicate that three intermediate phases, namely, the Mn3Sn, Mn,Sn, and MnSn, phases, exist at high concentrations of tin. However, so far the proper phase equilibrium has not been established at the manganese-rich end and very little data is available for the composition range between pure manganese and Mn3Sn. Moreover, earlier investigators differ in their opinion about the exact composition range at which the Mn3Sn and Mn,Sn phases appear and some doubt has been cast by some investigators3 regarding the structure of Mn3Sn phase which has been reported to be isotypic with Ni3Sn (Mgscd type) structure. In this investigation an attempt has been made to establish the proper phase equilibrium between pure manganese and Mn + 50 at. pct Sn composition in the temperature range of 500" to 1000°C. PROCEDURE The raw materials used were from three different sources. For exploratory work five alloys containing 5, 10, 15, 20, and 25 at. pct Sn were prepared using 99.9 pct pure manganese and tin supplied by E. Merck & Co., Germany. The rest of the alloys and one more 25 at. pct Sn alloy were prepared using 99.9 pct Mn supplied by Gallard Schlesinger Chemical Mfg. Corp., U.S.A., and 99.999 pct Sn supplied by Semi Elements Inc., U.S.A. Weighed amounts of manganese and tin were melted in recrystallized alumina crucibles in an inert gas (argon) high-frequency induction melting furnace. By careful control of temperature and time of melting the losses were reduced to below 0.2 pct in all cases. Since the losses were very small, no attempt was made here to analyze the samples chemically. Alloys were wrapped in molybdenum foil and sealed in small evacuated fused silica capsules. The alloys were annealed at different temperatures, controlled within + l°C, for sufficiently long periods to attain proper phase equilibrium, and subsequently quenched in cold tap water. The annealing periods used at different temperatures were 15 days at 500°C, 7 days at 600°C, 5 days at 700" and 750°C, 3 days at 800°, 850°, and 900°C, 2 days at 968"C, and two alloys annealed at 968°C were reannealed for 10 hr at 1000° C. From each annealed specimen, a part was utilized for metallographic study while another piece was used for X-ray diffraction study. 1.0 pct HNO, solution and oxalic acid solutions of concentrations 0.05 to 1.0 pct were used for etching Mn-Sn alloys above and below the MnsSn composition, respectively. Since all alloys were brittle, X-ray specimens were prepared using the as-crushed -325 mesh alloy powders. Only one 25 at. pct Sn alloy powder was reannealed in an evacuated silica capsule at 800°C for 5 min and water-quenched. X-ray diffraction patterns . for the Mn3Sn phase with the as-crushed and the reannealed powders did not show appreciable change. Un-filtered iron radiation at 25 kv, 15 ma was used with either Norelco 114.6-mm-diam Debye Scherrer Camera (for phase identification) or Norelco 12-cm-diam symmetrical focusing camera (for lattice parameter determination of the 6 Mn phase). The estimated accuracy of lattice parameter determination for the focusing camera was * 0.001A. RESULTS AND DISCUSSIONS The results of metallographic and X-ray diffraction study made with different alloys are shown in Fig. 1. The variations in lattice parameter with composition for the p Mn and the Mn3Sn phases are given in Tables I and 11, respectively, and the lattice parameter as a function of composition for the p Mn phase is shown in Fig. 2. The lattice parameter of the p Mn phase increases with increasing tin content while for the Mn,Sn phase the data obtained from two two-phase alloys and one single-phase alloy indicate increase in a,, and decrease in c, parameters with increasing tin content. The results, Fig. 1, indicate that the solubility of

Jan 1, 1969

By J. P. Kerr, W. H. Cordell

Conditions in the oil and gas industry in Indiana were about the same in 1935 as in 1934. This is especially true of the old Trenton area and the Harrison County area where production was steady and almost no exploration and development took place. The past year has seen an increase in drilling activity and a decrease in oil and gas output in southwestern Indiana. In the state, 224 wells were completed in 1935, of which 48 were oil wells, 61 gas wells, and 115 dry holes. A few of these were old gas wells deepened to oil horizons. Twenty-six wells started during 1935 were not completed by Dec. 31. Approximately one-half the wells drilled were within proven areas. A relatively large number of wildcats, especially in Daviess, Pike and Gibson Counties, were in search of new gas supplies to supplant the diminishing resources in those counties. The decreased production of gas was due largely to the fact that existing supplies declined more rapidly than new fields could be brought on. The Alford field, in Pike County, which produced the bulk of the supply in 1934, was called on to do likewise in 1935, but was unable to respond sufficiently to keep up the yearly production for southwestern Indiana. During the last half of the year, the Oaktown field, Knox County, was connected with one of the principal pipe lines of the state, which helped to keep gas production above an unusual low. The decline in oil production was due almost entirely to proration during the first eight months of the year. The proration affected Daviess, Pike, Gibson, Sullivan and Vigo counties, which produce about three-fourths of the total for the state. After proration was lifted, the wells never quite reached the conditions existing before proration. The average daily production per well in Indiana is less than two barrels. The outstanding development in Indiana in 1935 was the drilling in the Oaktown field immediately before and after the laying of the 6-in. pipe line to the field. Almost without exception the wells came in with an open flow of two to four million cubic feet. At the end of the year, 26 wells were connected to the pipe line. Development of this field will

Jan 1, 1936

By J. P. Kerr, W. H. Cordell

Conditions in the oil and gas industry in Indiana were about the same in 1935 as in 1934. This is especially true of the old Trenton area and the Harrison County area where production was steady and almost no exploration and development took place. The past year has seen an increase in drilling activity and a decrease in oil and gas output in southwestern Indiana. In the state, 224 wells were completed in 1935, of which 48 were oil wells, 61 gas wells, and 115 dry holes. A few of these were old gas wells deepened to oil horizons. Twenty-six wells started during 1935 were not completed by Dec. 31. Approximately one-half the wells drilled were within proven areas. A relatively large number of wildcats, especially in Daviess, Pike and Gibson Counties, were in search of new gas supplies to supplant the diminishing resources in those counties. The decreased production of gas was due largely to the fact that existing supplies declined more rapidly than new fields could be brought on. The Alford field, in Pike County, which produced the bulk of the supply in 1934, was called on to do likewise in 1935, but was unable to respond sufficiently to keep up the yearly production for southwestern Indiana. During the last half of the year, the Oaktown field, Knox County, was connected with one of the principal pipe lines of the state, which helped to keep gas production above an unusual low. The decline in oil production was due almost entirely to proration during the first eight months of the year. The proration affected Daviess, Pike, Gibson, Sullivan and Vigo counties, which produce about three-fourths of the total for the state. After proration was lifted, the wells never quite reached the conditions existing before proration. The average daily production per well in Indiana is less than two barrels. The outstanding development in Indiana in 1935 was the drilling in the Oaktown field immediately before and after the laying of the 6-in. pipe line to the field. Almost without exception the wells came in with an open flow of two to four million cubic feet. At the end of the year, 26 wells were connected to the pipe line. Development of this field will

Jan 1, 1936

By Thomas A. Simpson

THE Birmingham red iron ore district in Jeffer-son County, north central Alabama, Fig. 1, is bounded on the northwest by the Warrior and Plateau coal fields and on the southeast by the Cahaba and Coosa coal fields. The area of study includes the ridge and valley between Red Mountain and Shades Mountain, Fig. 2, approximately 70 square miles extending from Homewood in the northeast to Greenwood in the southwest. The district is one of the most important producers of hematite in the United States, with an annual production of about 7 million tons.' The amount of hematite mined between 1870 and 1950 ranged from 6 to 16 pct of the nation's total annual production,' and the iron and steel products from blast furnaces in the Birmingham district supply the entire southeastern section of the country. Most of the mining in the Birmingham district is from slope mines along the outcrop of the ore on Red Mountain, such as Red Ore, Muscoda, Spaul- ding, and Sloss. The Pyne and the Shannon are the shaft mines of the area. The Shannon mine of Republic Steel Corp., in the central part of the area under study, is in Shades Valley at the foot of Shades Mountain. The Pyne mine of Woodward Iron Co. is 2 miles east of Readers Gap in Shades Valley. The hydrology problem has become more prevalent as mining in the area has progressed downdip. An extensive exploratory diamond drilling program is necessary to determine areas where water pressures and abnormal flows are excessive. This operation, added to higher pumpage rates, has greatly increased the costs of ore extraction. In November 1952 the U. S. Geological Survey began a detailed study of occurrence and movement of ground water in the iron mining areas of the Birmingham district. The study is a part of a small-scale but nationwide program to develop data that will be of help to the mining industry in solving mine water problems. The area of the study, in the Ridge and Valley province of the Appalachian system, Fig. 1, is a series of alternate ridges and valleys trending northeast. The principal ridges are Red Mountain, altitude about 1000 ft, and Shades Mountain, about 1100 ft. Shades Valley is between these two ridges, and its lowest point is about 480 ft. Shades Moun-

Jan 1, 1956

By M. R. Geer, Franklin T. Davis, H. F. Yancey

COKE with low phosphorus content is required by some of the electrometallurgical and chemical plants recently attracted to the Pacific Northwest by the hydroelectric power available from Bonneville and Grand Coulee dams. Shipping such coke into the area from eastern points involves a high freight charge, and during wartime consumes precious rail and ship-bottom space, so it is highly desirable to produce coke from the coking coals of Washington to meet the requirements of these industries. Although coke has been made from Washington coals since 1884, little has been known about their phosphorus contents or about the extent to which phosphorus could be reduced by cleaning. An investigation was undertaken, therefore, to determine the manner in which phosphorus occurs in the coking coals of Washington and its amenability to removal by ordinary coal-washing methods. PREVIOUS WORK Phosphorus is a deleterious element in coke used for numerous metallurgical processes, including the production of pig iron, yet comparatively little published information is available on the occurrence and elimination of phosphorus in any of the coals of this country. A variation from 0.009 to 0.062 per cent phosphorus in various horizons of the Pittsburgh bed in the Connellsville region of Pennsylania has been reported,1 and a reduction in phosphorus content from 0.020 per cent in the raw coal to 0.018 per cent in the washed coal was obtained in washing coal from the same bed in the Pittsburgh area;2 the latter figures represent average analyses for a year's operation of the washery on about 800,000 tons of coal. A reduction in phosphorus content from 0.018 to 0.011 per cent in washing coal from the Pittsburgh bed at another washery was observed, and the same report provides data on the phosphorus reduction obtained by separating 10 other coals on a bath of 1.35 specific gravity.3 European investigators have been especially active in correlating phosphorus content with petrographic analysis; fusain and durain generally contain the highest percentage of phosphorus, but this relationship is not universal.4 Some of these investigators have found that phosphorus is removed in the coal-washing process,5 but others have observed that the clean coal contained as much or even more phosphorus than the raw coal.6

Jan 1, 1944

By B. A. Cheadle, K. P. Steward

Axial tensile, ring tensile, closed end burst, and free end burst tests were done at room tempe.vature and 300°C on three batches of Zircaloy-2 sheathing zuith different textures. Knoop hardness tests were also done on all batches. The mechanical properties of the tubes were largely dependent on the percentages of cold work, but were also markedly affected by the textures, particularly with respect to deformation behavio'r. The deformation behavior observed confirmed Picklesimer's predictions, zuhereas Knoop hardness results could be correlated with texture and yield strength anisotropy after the ,method of Wheeler and Ireland. From the mechanical properties, and from efjectiue strain values deterrlzined at the fractures using a photoqid technique, it zuas concluded that tubing witlz a single preferred orientation of radial basal poles best combines strength and ductility for any given deqee of cold work. THE mechanical properties required in collapsible Zircaloy-2 fuel sheathing for water-cooled power reactors are strength to resist wrinkling deformation by coolant pressure and ductility to accommodate a small amount of deformation in service without rupturing. Zircaloy-2 tubing during fabrication develops pre- ferred orientations of the a Zr grains due to aniso-tropic deformation behavior, and these textures markedly affect mechanical properties. Picklesimer' had predicted the deformation behavior of tubes with various textures, but the texture required to provide the optimum strength and ductility for a given degree of cold work has not been reported. To investigate this problem, tests at three transverse to axial stress ratios were done at room temperature and 300°C on three batches of Zircaloy-2 tubing covering a wide range of textures and percentages of residual cold work. Knoop hardness values were also measured to correlate with preferred orientation and yield strength anisotropy after the method of Wheeler and relland.' 1) MATERIAL For this investigation, three batches of tube-reduced tubing were chosen from the Zircaloy-2 sheathing produced for the Douglas Point Reactor. Individual tubes were 191/2 in. long, 0.600 in. OD, and 0.0165 in. nominal wall thickness. The identities of the batches, together with their textures, are shown in Table I. The tubes had the normal Zircaloy-2 composition3 of 1.5 wt pct Sn, 0.3 wt pct Fe, Ni, Cr combined with the following oxygen concentrations: Batch VII 1140 to 1390 ppm 0 Batch VIII 1400 to 1750 ppm 0 Batch IX 880 to 1320 ppm 0

Jan 1, 1968

By R. Dawson Hall

The stresses in the simplest structures are often those we find most difficult to analyze. The most complex condition in mine stresses is found in simple tunnels where the roof, the sides, and the floor are a monolith. The functions of the parts are like the parts themselves not distinct and spccialized, and the problems to be solved are like those in a metal structure with riveted joints or a redundancy of bars. This difficulty explains perhaps why the condition has not been treated. But just because it cannot be discussed in its entirety is no reason why it should be treated as an action of parts with spccialized functions as a roof beam with supports and a foundation. The problern cannot be ignored on the ground that it is not of sufficient importance to warrant careful consideration, because conditions of complete monolithism, of which the tunnel is the type, are found materially unchanged in room-and-pillar and in longwall work. This unity between roof, sides, and floor, which to the coal miner is a difficult conception, really deserves a scientific appellation, and perhaps holoid (from holos, whole, and eidos, form) will serve the purpose as well as any other. In a simple tunnel the roof, the sides, and the floor form integral parts of one and the same structure, and the distortion of one cannot be conceived without a consequent strain in the others. Thus when the roof of the tunnel droops by reason of its weight, the upper parts of the sides are drawn in becausc they are integrally connected with the roof and must approach each other whenever, by the sagging of the roof, the distance between any two points in it is diminished. (See Fig. 1.) Thc sides in their turn operate on the floor of the holoid structure, producing a tensile stress. The writer has always been impressed with the value of soap as a means of illustrating the action of mine stresses. With that idea in mind' a cake of naphtha soap measuring 43/8 by 2¼ by 19i in. was taken and a tunnel was made through it 13/4 in. long, 21/2 in. wide and 1¼ in. high. (See Fig. 2.) A load was then placed at the mid-span of the tunnel. Eventually, the upper bar, or "roof," broke at the

Jan 1, 1916

By Nathaniel Arbiter, Arthur F. Taggart

THE chemical reaction occurring in collection of nonmetallic minerals with amine-type collectors was early postulated by students of flotation phenomena to be metathesis between the mineral and the collector, involving exchange between the amine-bearing (aminium) ion and the cation of the mineral, and formation at the mineral surface of an oriented film of the amine salt of the mineral anion. Qualitative evidence of exchange has been obtained on several occasions at Columbia. Thus 1000 c.c. of a solution containing 495 mg. of laurylamine hydrochloride was shaken 17 min. with 100 grams of barite and ground in a porcelain mill to pass a 200-mesh screen; the mixture was then set aside for 48 hr. Filtrate therefrom analyzed 476 mg. per liter of laurylamine hydrochloride. There was no substantial loss of chloride ion (78.4 mg. per liter in the original; 74 in the filtrate). No successful analyses were concluded for barium ion. Earlier, confessedly rough work with scheelite indicated a solution gain in Ca++ equivalent to about one-half the aminium ion lost. Real quantitative proof of the exchange, in the form of an established stoichiometric balance, is unknown to the authors. The data of the present paper, however, obtained from experiments designed on the basis of the exchange hypothesis, constitute strong evidence of its truth, and at the same time point the way to economic utilization of the expensive nitrogen-bearing collectors in concentration of the low-priced nonmetallic minerals. The basic postulate underlying the experiments performed was that, if the collecting reaction is of the type [R+ + Y- + MX =± RX + M+ + Y¬] where R = aminium ion, Y = the anion of the amine salt, and M and X are, respectively, the cation and anion of the mineral, the reaction should obey qualitatively the implications of the massaction and solubility-product laws. This is to say that coating and collection should be aided by the addition to the solution of either ion (R+ or X-) of the collector-coating compound, and hindered by the addition of either of the ions M+ or Y-. Experimental work comprised determination of (1) the relative solubilities of the laurylammonium salts of a variety of nonmetallic-mineral anions; and (2) the contact angles1 of various minerals in solutions containing different concentrations of the postulated controlling ions. Semiquantitative flotation tests were run with barite as checks on the diagnostic character of the contact angles. The amine

Jan 1, 1944