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By S. Pearson, L. Rotherham

Measurements have been made of the variation of internal friction with temperature for spectroscopically pure silver, and for o series of solid solutions of silver with cadmium, indium, and tin, using a Ke-type torsion pendulum apparatus. Some experiments have also been made to investigate the effect of nonmetallic impurity on grain boundary relaxation in silver. The effect of the alloying elements is to increase the grain boundary viscosity, and to raise the activation energy for grain boundary relaxation from 22,000 cal per mol for pure silver to 43,000 cal per mol for the solid solutions; the same value being obtained, within the limits of experimental error, for all the alloying elements and solute concentrations investigated. Results of the experiments show exactly the same trend as those obtained previously for a similar series of copper solid solutions. They are in agreement with the general theory of grain boundary relaxation developed by Zener and Ke, but do not seem to be in agreement with either of the mechanisms so far put forward to explain grain boundary slip. EXPERIMENTS described in this paper were made as part of an investigation into the effect of alloying elements in substitutional solid solution on grain boundary viscosity, measured by the internal friction method developed by Ke.&apos; The apparatus and experimental procedure have already been described.&apos; Preliminary work was done with spectro-scopically pure silver. Experimental Work Materials Used—All the materials were supplied in the form of % mm diam wire by Messrs. Johnson Matthey and Co. Ltd. The silver and all the alloying elements used were spectroscopically pure. Composition of the alloys is given in Table I. They were all melted and chill cast under the same conditions as the copper alloys. The ingots were rolled to 1/4 in. sq rod with intermediate annealing at 600°C in an atmosphere of cracked ammonia when necessary. These rods were then drawn to wire by standard procedure with intermediate bright anneals at suitable steps in the drawing operations. Specimens from the annealed wires were sectioned longitudinally. mechanically polished, and examined under the microscope. They were then etched and reexamined. Grain sizes were reasonably uniform for all wires, and no traces of a second constituent were observed. The wires were weighed before and after testing so as to measure any loss of the alloying element due to evaporation. The loss was less than the accuracy of measurement—< 0.1 pct of the total weight— for the Ag-In and Ag-Sn alloys, but appreciable loss of weight occurred in the case of the Ag-Cd alloys. The percentage loss is given in Table 11. X-ray diffraction photographs were taken of all thc wires after test to determine whether there was any marked preferred orientation. Results of the examination are given in Table 111. Experiments on Spectroscopically Pure Silver-— Experiments were made on specimens in which the grain diameter was small relative to that of the wire, and on one specimen in which the grains were grown by the usual strain-anneal method to extend across the full diameter of the wire. These large grained specimens will be referred to as single crystal specimens. The wires were annealed for 11/2 hr at 700°C, and experiments were made at two frequencies of vibration, 1.5 and 0.4 vibrations per sec. The variation of internal friction with temperature is shown in Fig. 1. Experiments on a second small grain specimen gave approximately the same results as for the first wire. It will be seen from Fig. 1 that the peak in the curve for the small grained wire, which is presum-

Jan 1, 1957

By Allan Martin, R. A. Swalin

Diffusion rates of manganese, aluminum, titanium, and tungsten in nickel were measured at temperatures between 1100° and 1300°C. Activation energies, Q, and values of the frequency factor, Do, were calculated for each system. Values of Q were found to be within 15 pet of that for self-diffusion of nickel in agreement with present theories of diffusion. ONE of the most interesting problems in diffusion concerns factors governing the order of diffusion coefficients of various solutes in a common solvent metal at low solute concentrations. An early suggestion by Rhines and Mehl&apos; was that diffusion coefficients might each approach that of the self-diffusion coefficient of the solvent itself. Later Thomas and Birchenall&apos; pointed out correlations between the order of the diffusion coefficients and the freezing point depressions of the solvent by the various solutes. Other correlations have been sought. To settle this question it seems likely that much more data will be needed and, in particular, data collected at low solute concentrations. This type can be obtained by special analytical techniques as well as by use of radioactive tracers. The following study was made of diffusion of manganese, aluminum, titanium, and tungsten in a common solvent, nickel, at relatively low solute concentrations: 1—Production of alloys of nickel with manganese, aluminum, titanium. and tungsten at concentrations of the order of 1 atomic pet. 2—Use of pressure-welded diffusion couples in cylindrical form. 3—Diffusion anneals in the temperature range of 1100" to 1300°C. 4—Lathe sectioning of the diffused couples. 5—Spectrophotometric analyses of lathe turnings for the solute being studied. 6—Calculation of the diffusion coefficient for each of the solutes as a function of temperature. 7—Interpretation of results with current theories of diffusion. Experimental Work Materials—Two types of nickel were used in this research. The grade designated as Vacuum melted Mond nickel was used for all diffusion systems except the Mn-Ni system for which the Vacuum melted electrolytic nickel was used. Analyses of the two grades are given in Table I. The manganese used in making alloys was 99.9 + pet pure, aluminum 99.99 pet pure, titanium 99.9 pet pure, and tungsten of C.P. grade powder. Alloys used in this investigation were prepared by melting in vacuo or under a low pressure of argon. After melting, all heats except those of nickel-manganese were poured into a cylindrical copper mold 3 in. long and 1 in. ID. In the case of nickel-manganese, the alloys were solidified in the melting crucible. For nickel-aluminum heats alumina crucibles were used and for all other heats, zirconia crucibles.

Jan 1, 1957

By John T. Norton

N order to attempt to arrive at a better under-Jl standing of the whole basic problem of sintering, these remarks will serve as an introduction for discussion that is included and will, perhaps, help to isolate specific questions which need to be answered or to suggest some definite avenues of investigation which should be followed. To bring some sort of logical order into the presentation, I will consider the various types of interaction between the metal to be sintered and the atmosphere which surrounds it, depending upon whether the phenomena are essentially chemical or physical in nature. For example, when the only necessary criterion for the satisfactory sintering of a certain powder is the removal of an oxide skin, then the problem of choosing a suitable atmosphere is primarily chemical; however, if a special surface condition as a consequence of the oxide skin removal is necessary for particularly effective sintering, then the problem becomes a physical one. Of course, the two aspects overlap considerably, but it may be possible to make a distinction in principle if not in practice. The chemical characteristics of the phenomena will be emphasized, since these are the better known. Metal-gas reactions involved in sintering are controlled primarily by the thermodynamics of the processes involved. In which direction will a reaction go and how far before it stops? The answer is to be found in the magnitude of the free energy change associated with the reaction. If a constituent is to be removed from the specimen as completely as possible or if a constituent is to be formed in the specimen as completely as possible, then one chooses conditions which are far from equilibrium so that the reaction is driven toward completion. On the other hand, if the composition is to be maintained at a desired value, then conditions are adjusted as closely as possible to the equilibrium point. This aspect of the problem is susceptible to quite precise analysis, provided, of course, that the significant reactions can be recognized and the required thermodynamic data are available. Conversely, if one asks how fast the reaction goes or how far it proceeds in a given time, the answer is frequently much more difficult to answer in quantitative terms. Yet the rate-con trolling factors of the reactions may be of primary importance in the success of a particular operation, especially where competing processes are at work. Both equilibrium and rate factors must be understood if a clear picture is to be obtained. For instance, in a process for carburizing titanium dioxide, is the difficulty of obtaining a stoichiometric Tic due to a true limitation of the equilibrium or simply to a very slow rate of reaction? An example of this appears in the work of Kalish and Mazza.&apos; They showed that the oxygen content of sintered iron compacts was lower when sintered in pure hydrogen than in the case where the hydrogen was diluted with either argon or nitrogen. The equilibrium oxygen content of the iron would be the same in the two cases, since it is determined by the ratio of the partial pressures of water vapor and hydrogen and this pressure ratio is unchanged by dilution. The rate of oxygen removal, however, under the conditions of a constantly replaced furnace atmosphere, depends upon diffusion and thus upon the concentration of hydrogen in the furnace atmosphere. Possibly the clearest way to illustrate the interplay of these two factors is to consider in more detail some of the typical metal-gas reactions. Adsorbed Gases It is common experience that fine metal powders with their very large surface areas often contain large quantities of gas. This gas, which results from exposure to air or perhaps from some step in the

Jan 1, 1957

By G. Derge, Ling Yang, G. M. Pound

The specific conductance and its temperature dependence were measured over the entire composition range of the molten Cu2S-CuCI system. At a typical temperature of 1200°C, 10 rnol pet of the ionically conducting CuCl reduced the specific conductance from about 77 ohm-lcm-l for pure Cu2S to about 32 ohm -1cm -1, and 50 mol pet CuCl reduced the conductance to that for pure CuCI—about 5 ohm 1cm1. The nature of electrical conduction in molten Cu2S, FeS, CuCI, and mixtures was studied by measuring the current efficiency of electrolysis at about 1100°C. The Cu2S, FeS, and mattes were found to conduct exclusively by electrons, but addition of 1 5 wt pet CUS to Cu2S produces a small amount of electrolysis. Addition of CuCl to Cu2S suppresses electronic conduction, and ionic conduction reaches almost 100 pet at a CuCl concentration of about 50 mol pet. These facts are interpreted in terms of electron energy level diagrams by analogy to the situation in solids. RESULTS of electrical conductivity studies on molten Cu-FeS mattes as a function of composition and temperature have been reported.&apos; The specific conductances ranged from about 100 ohm-&apos; cm-&apos; for pure Cu2S to 1500 ohm-&apos; cm-1 for pure FeS. This is in sharp contrast with the low specific conductance of molten ionic salts for which the transfer of electricity is by migration of ions in the field. In general, these ionically conducting molten salts, such as NaC1, KC1, CuC1, etc., have a specific conductance of the order of magnitude of 5 ohm-&apos; cm-&apos;. It was concluded on the basis of this evidence that molten FeS and Cu,S exhibit electronic conduction. Pure molten FeS has a small negative temperature coefficient of specific conductance, resembling metallic conduction, while pure molten Cu2S has a small positive temperature coefficient, resembling semi-conduction. The molten Cu2S-FeS mattes follow a roughly additive rule of mixtures, both with respect to specific conductance and temperature coefficient. Savelsberg2 has studied the electrolysis of molten Cu2S and Cu2S + FeS. He concluded that while molten Cu2S is an electronic conductor, there is some ionic conduction in molten Cu2S + FeS3 owing to the formation of the molecular compound 2Cu2S.FeS and its dissociation into Cu1 and FeS2-1 ions. The present work does not verify his results. Chipman, Inouye, and Tomlinson" have studied the specific conductance of molten FeO and report a high specific conductance, about 200 ohm-1 cm-1 of the same order of magnitude as that found for molten mattes, and a positive temperature coefficient. They interpret these results in terms of p-type semiconduction in the ionic liquid by analogy to the situation in solid FeO.1 imnad and Derne&apos; detected appreciable ionization in molten FeO by means of electrolytic cell efficiency measurements. In order to verify the conclusion that electrical conduction in molten Cu2S and mattes is electronic, and to gain further insight into the structure of molten sulfides, the following investigations were carried out in the present work: 1) The specific conductance, s of the molten system Cu2S-CuC1 was measured as a function of temperature over the entire composition range. As discussed later, molten CuCl is an ionic substance. It was thought that if molten Cu2S were simply ionic in nature, addition of small amounts of CuCl might not have a catastrophic effect in lowering the high conductance of the Cu2S. On the other hand, if much electronic conduction occurs, addition of the ionic CuCl should have a large effect in destroying the electronic conduction. 2) The electrolytic cell efficiency of the following molten systems was measured at about 1100°C in specially designed cells: Cu3; Cu2S + FeS, 50:50 by wt; FeS; Cu2S + CuS, 15 wt pet; Cu2S + CuC1, 5.9 to 46.4 mol pet; and CuC1. This gives a direct measure of the fraction of current carried by ions in these melts. Further, the cell efficiency, extrapolated to zero ionic current, is given by cell efficiency = (s leasile + s elexstronic). [1] s lucile for molten CulS would be expected to be no greater than that for molten CuC1, whose s lonle is about 5 ohm-&apos; cm-1, as will be seen in the following. u,.,,.,.,.......for molten Cu,S is of the order of 100 ohm-&apos; cm-&apos;.&apos; Thus, a large increase in cell efficiency from 0 to values of 10 to 100 pet upon addition of CuCl to Cu2S would indicate destruction of the electronic conductance. Conductance Measurements Experimental Procedure—The apparatus and experimental method were the same as those described in detail in connection with the study of electrical conduction in molten Cu,S-FeS mattes.&apos; A four terminal conductivity cell and an ac poten-

Jan 1, 1957

By Ulrich H. Roesler

RECENTLY, C. Zener1 published a new thermo-dynamic treatment of the a/y transformation in iron alloys. His interpretation differs from the previous theories2-0 ainly through the separation of the free energy difference, Ga—G, into two additive

Jan 1, 1957

To finalise the arrangement and details of the headframe to be erected over the new No. 3 Shaft, the haulage and winding equipment requirements were first determined, then tentative designs were prepared to cover the needs of general shaft servicing work for men and materials, mullock and ore handling, and the probable requirements of a breaker station to be built adjacent to the headframe, which would provide for the crushing of the run-of-mine ore down to a size which would be suitable for feeding on to the concentrating mill.

Jan 1, 1957

By S. S. Clarke

This paper on methods and costs of mining at the Westside mine, in the Tri-State zinc-and lead-mining district (Missouri-Kansas-Oklahoma), is one of a series being prepared by the Bureau of Mines on mining practices, methods, and costs in various mining districts of the United States. Methods and equipment used in drilling, loading, and underground transportation have changed radically since the latest Bureau of Mines publications2/ on mining methods in the district were published more than 20 years ago. More efficient methods and machines have been developed in order to maintain low operating costs in the face of rising labor and supply costs and lower grade ore. The rate of conversion to mine mechanization was disappointing at times; local conditions required the development of special equipment, and available rock-moving machines had to be remodeled and strengthened.

Jan 1, 1957

By O. Mellgren, A. M. Gaudin, P. L. De Bruyn

The adsorption density of ethyl xanthate on pyrite was determined as a function of xanthate concentration. Surface preparation of the mineral appears to have asafunctionsome effect on the subsequent adsorption process, A monolayer of xanthate on the surface is exceeded only in presence of oxygen. The effect of OH- , HS- (and x and CN- S=)and on the amount of xanthate adsorbed was investigated. Competition between OH- and X- (xanthate) ions for specific adsorption sites is indicated over a wide pH range. IN the flotation of sulfide ores, xanthates are most commonly used to prepare the surface of the mineral to be floated so that attachment to air takes place. The quantity of agent required to make the mineral hydrophobic is usually very small, of the order of 0.1 to 0.25 lb per ton of mineral. Details of the mechanism of pyrite collection are for the most part unsettled. Adsorption of collector has long been believed to involve an ion exchange mechanism as demonstrated for galena&apos; and for chalcocite.2 In the work on chal-cocite it was also demonstrated that a film of xanthate radicals unleachable in solvents that dissolve alkali xanthates, copper xanthate, or dixanthogen was formed at the surface of the mineral. The unleachable product increased with increasing addition of xanthate up to a maximum corresponding to an oriented monolayer of xanthate radicals. Pyrite is extremely floatable with xanthate if its surface is fresh.9 ut the floatability decreases rapidly as oxide coatings increase in abundance. Pyrite shows zero contact angle when in contact with ethyl xanthate solution at pH higher than about 10.5;4 at neutrality, a contact angle of 60" is obtained at a reagent concentration of 25 mg per liter. Alkali sulfides and cyanides are pyrite depressants. In this study of pyrite collection the writers have sought to relate measured xanthate adsorption to the method used in preparing pyrite, to the presence or absence of oxygen, to concentration of hydroxyl, hydrosulfide, sulfide, and cyanide ions. The principal experimental tool has been radioanalysis," " using xanthatcx marked with sulfur 35. Experimental Materials Pyrite: Unlike most sulfides, pyrite is a poly-sulfide. The structure given by Bragg7 resembles that of sodium chloride, the iron atoms corresponding to the position of sodium and pairs of sulfur atoms corresponding to the position of chlorine. The edge of the unit cell in pyrite is 5.40 A and in halite 5.63 A. The S-S distance in pyrite is 2.10 A; the Fe-S distance, 3.50 A: and the Fe-Fe distance, 3.82 A. Natural pyrite from Park City, Utah, was used in this investigation. Pyrite 1 was obtained by hand picking pure crystals. Pyrite 2 and Pyrite 3 were obtained from finer textured crystalline material containing inclusions of silicates. The same cleaning technique was utilized for the preparation of Pyrite 2 and Pyrite 3, whereas a different cleaning technique was used for Pyrite 1. Pyrite 1 was prepared as follows: The crystals were ground in a porcelain ball mill and the 200/400 mesh fraction was separated by wet screening with distilled water, followed by washing for 1 hr with deoxygenated distilled water acidified with sulfuric acid to pH 1.5. The acid was removed by rinsing with deoxygenated distilled water on a filter until a pH of 6.0 was reached in the effluent. This filtration was carried out under nitrogen. The sample was then dried in a desiccator under nitrogen. The period of time for which this pyrite sample was in contact with water containing oxygen was about 4 hr. The specific surface as determined by the BET gas adsorption method was 582 cm2 per g. Final material assayed 53.12 pct sulfur and 46.5 pct iron (theoretical, for FeS,: S, 53.45 pct; Fe, 46.55 pct). After crushing, Pyrite 2 and Pyrite 3 were washed with 1 M HCl. rinsed, and fed to a laboratory shakinq table to remove the small amount of silicates. The concentrate obtained was ground in a laboratory steel ball mill. The 200/400 mesh fraction was separated by classification in a Richards hindered settling tube. This fraction was then given a final wash with 0.1 M HCl and deoxygenated water was filtered through the sample. The final effluent showed a conductivity equivalent to that of a solution having a salt concentration of 0.3 ppm. Aqueous hydrogen sulfide solution was then added to the sampln (about 100 ml saturated H,S solution to about 1000 g pyrite under a few hundred milliliters of water) which was stored wet under nitrogen. The sample stored in this manner showed no indication of formation of iron oxides, whereas iron oxides appeared

Jan 1, 1957

A calibration of the Frantz isodynamic magnetic separator relates the current in the electromagnet and the transverse slope of the chute to the specific susceptibility at which separation is being effected. In addition to providing a rapid measure of the specific susceptibility of minerals and composite grains, the calibration provides a guide to operation of the Frantz isodynamic separator for mineral separation, and to the nature of composite grains. The most sensitive magnetic separation is obtained by using the highest practicable current and transverse slope, and the lowest practicable longitudinal slope.INTRODUCTIONProbably all minerals have a magnetic susceptibility measurable by sensitive techniques. However, magnetic separation between minerals which have low but different specific susceptibilities, and which for many purposes are considered essentially non-magnetic, has only become practicable with the development of the Frantz isodynamic separator.The construction and principle of this highly sensitive separator has been described by S. G. Frantz as an appendix to a description by &apos;Gaudin and Spedden (1943) of its application to the separation of sulphides constituting mill products.Various publications (e.g. Hess, 1949, Hutton, 1952) refer to its use in separating the mineral constituents of rocks, ores, and unconsolidated sands.As used in this study the Frantz isodynamic separator consists of a vibrating chute mounted centrally between the pole pieces of an electromagnet (Fig. 1). This unit may be inclined in any direction by the universal mounting, and the electromagnet current is continuously adjustable from 0 to 1&#183;5 amperes.

Jan 1, 1957

By B. F. Peters, J. Gordon Parr, E. R. Macgregor

A SERIES of seven hypoeutectoid alloys, up to 18.2 atomic pct Mn, was made by the levitation melting technique. The loss of weight on melting was considered to be entirely due to volatilization of manganese, and compositions were computed on this basis. Filed samples (—200 Tyler mesh) were helium quenched from 1000°C after soaking for 5 min by a technique already described.&apos; Quenched Alloys -Assessments of the amounts of a phase produced and the hardness of the quenched alloys are summarized in Fig. 1. The experimental techniques and calculations involved have been described previously. The amount of a decreases as manganese content increases, until at 10.6 pct Mn only a trace of a&apos; is observed. Previous

Jan 1, 1957

By R. M. Treco

THE purpose of this work has been to investigate recrystallization characteristics of zirconium after cold working and annealing. In order to do this, hafnium-contain ing crystal bars of Foote Mineral Co. iodide zirconium were selected for high purity. maximum diameter (about ½ in.), brightness of surface, and absence of core wire. A typical lot analysis is shown in Table I. In order to obtain uniformity of starting material, all bars were cold-swaged to 0.310 in. diam, annealed for 2 hr at 1000°C, and furnace cooled.

Jan 1, 1957

By John M. Campbell, W. E. Portman

A series of correlating charts have been prepared to enable the field engineer to predict the amount of stock tank fluid produced by stabilization of first stage separator fluid. The charts shown are particularly convenient for estimating the relative effect of temperature and pressure in economic studies. Further work is planned to investigate the factors affecting stage separation&apos; yo supplement this preliminary work. The direct correlation of separation variables is dictated as a convenience to eliminate the trial and error calculation necessary when using the standard flash vaporization equations. These are obtained by a material balance using the equilibrium vaporization ratio K, and have appeared in the following, or similar. form many times in the literature. where La = mols of any component n in the separator liquid Ko — equilibrium vaporization ratio for any component at separator pressure and temperature Fa = mols of any component n in the feed Vn = mols of any component n in the vapor V = total mols of separator vapor These equations may of course be effectively and accurately solved by use of digital and analog computers. However, these are not usually readily available in field offices and the need often arises for fast results during routine operational problems. Consequently, many methods have been devised in an attempt to simplify the basic calculation.2-14 The methods proposed are generally satisfactory, but do not eliminate trial and error methods and the necessity of subsequent calculations to obtain the answer in volume terms. The purpose of this work. therefore, was to develop accurate charts that would give the result directly in gallons. When using stage separation the recoveries would be lower than those shown, for stabilization usually gives about 95 + per cent recovery on the potential stock tank components in the separator liquid. The recoveries are shown in terms of a 14 psi Reid Vapor Pressure product which has a true vapor pressure of 14.7 psia at 98°F. Consequently, this product represents a stable stock tank liquid under normal storage conditions. To estimate natural gasoline re- coveries by stabilization the volume shown may be multiplied by 1.20 for 18 Ib RVP natural gasoline and 1.36 for 26 lb RVP natural gasoline. PROCEDURE The five analyses shown in Table 1 were chosen since they were representative of wellstream compositions often found and had almost the same propanes plus liquid content, expressed in gallons per 1,000 std. cu ft of wellstream. The distribution of the components though is widely variant. A temperature range of 0-100°F. and a pressure range of 200 to 1,250 psia was chosen inasmuch as most separations fall within these limits The K values used were modified values of those originally published by Katz and Hachmuth.&apos; In the range chosen these have generally given good results when predicting fluid recoveries. The choice was somewhat arbitrary, for the authors&apos; personal experience has shown that

Jan 1, 1957

By Wilbur A. Haley

One of the purposes of the investigation was to determine and report on how coal augers are used to mine bituminous coal that is near outcrops and may not be mined otherwise by any other present-day method. Such increased overall recovery results in the conservation of coal resources. Other reasons for the investigation were to determine and report the production rates of such operations and the types of equipment used. Auger mining of coal as a means of coal recovery supplementary to strip mining has been introduced and developed since World War II. This type of coal mining has grown rapidly, and bituminous-coal production by auger mining has been estimated at 6,000,000 tons in 1955. Mines were selected for study to give reasonably representative information on auger mining in different types and thicknesses of coal beds in different geographic areas and on different types and sizes of equipment operated under various conditions. This report is based on field studies of 8 auger-miming operations in Pennsylvania, West Virginia, and Ohio and in 5 different coal beds. Operations were observed in active strip mines, in strip mines reopened for auger mining, and along benched coal-bed outcrops. At the time of this study, no augers were reported to be operating in underground mines. The diameters of holes drilled ranged from 26 to 52 inches, and the lengths of holes ranged up to 208 feet. At some operations auger holes often penetrated abandoned underground mine workings.

Jan 1, 1957

By J. B. Rosenbaum

This report presents new findings and consolidates previously published data to provide a single reference containing a concise and comprehensive description of the Bureau&apos;s work on electrolytic chromium. Two separate systems for electrolytic-chromium recovery were developed, one designated as the oxidized system the other as the reduced system. The electrowinning of chromium metal follows the dissolution of chromium from the ore or from ferrochrome and its separation from gangue and metallic impurities. Chromite was first solubilized by pressure digestion at slightly elevated temperatures in an oxidized acid solution using Na2Cr2O7 as an oxidizing agent. Later it was found that a sodium-free electrolyte was preferable, using return-cell anolyte containing H2SO4 and Cr03 as the oxidizing agent. Gangue materials were separated from the soluble metallics by filtration; and, after the Cr+3 had been stabilized, the metallic impurities were separated as crystalline ammonium salts by vacuum crystallization.

Jan 1, 1957

By I. Havenaar

EXPERIMENTAL DATA In an article by C. K. Ferguson and J. A. Klotz,1 experiments on the filtration of drilling muds under borehole conditions are discussed. Experimental data on mud filtration through the wall and the bottom of the hole are presented. From the data on bottom-hole filtration it was concluded that the filtrate does not flow freely into the formation, but that the pores of the formation are plugged by the mud. A quantitative interpretation of the data can be civen, by using a formula for bottom-hole filtration, dehved below. This formula is based on the following assumptions, 1. Each time a blade of a drag bit, or a cone of a roller bit, moves along the bottom of the hole, the mud cake is completely removed. 3. A new mud cake is immediately formed on the freshly produced surface, and losses of "whole" mud into the formation are negligible (this is equivalent to an immediate plugging of the pores). 3. The filtration of the mud on the bottom of the hole follows the classic law: V = A +1—(Eq. I), where t is the time required to yield a volume of filtrate V, A is the surface area of filter cake, and C is a constant. The application of this equation means that any eroding effect of the mud stream on the mud cake is neglected. The formula for the calculation of the volume of filtrate, Q,, flowing in one second through the hole bottom (diam. d cm), when using a bit with n cones or blades rotating at a rate of rn revolutions per second, is derived as follows: The mud cake is formed on the bottom of the hole in the time t =1; the filtrate volume V which passes n through the bottom In this time 1s given by Eq. 1: After1/nmsec the mud cake is removed. In one m second this process takes place nm times. Therefore the volume of filtrate, obtained in one second is given by This equation has now been applied to the experiments of Ferguson and Klotz. The constants C were derived by means of Eq. 1 from the API filter losses of the muds used by the authors (t = 1,800 sec; A = 45.16cm2). A three-cone bit was used (n = 3) at 90 rpm (m = 1.5). The calculated figures are compared with the experimental data in the table below. The calculated values of Q, are usually lower than the experimental values. This may be due to the following causes. 1. The value of C used in the calculation is based on the API filter test (filtration pressure of 100 psi), whereas the experimental data were obtained with a filtration pressure of 200 psi. Although the effect of the pressure on C is not large, C decreases somewhat with increasing pressure, and this leads to a higher filtration rate. 2. Mud losses and the eroding action of the mud stream on the cake are not entirely negligible. 3. The values of Q, derived by Ferguson and Klotz from their experiments are too high, because of their assumption that all pore liquid within the formation drilled is picked up by the drilling mud. It is found, however, that the calculated values of Qf, except in the case of oil base muds, are of the right order of magnitude. ACKNOWLEDGMENT The author wishes to thank the management of the Koninklijke/Shell-Laboratorium, Amsterdam, for permission to publish this note.

Jan 1, 1957

By D. W. Levinson, L. F. Mondolfo, N. A. Gjostein

MANY investigations are reported in the literature on the age hardening of Al-Mg-Zn alloys but most of them are concerned mainly with mechanical property changes. The present investigation was started to determine the structural changes in an AlMgZn alloy. The alloy composition was chosen in the existing phase diagram" so as to lie on the quasi-binary section Al-(AlZn)Mg Actually, it was found that the diagram as published was inexact at the lower temperatures and that the phase in equilibrium with aluminum at the lower temperatures is not the ternary compound. Technique The alloy used for the investigation was prepared from high purity materials and the resulting composition as determined by chemical and spectro-graphic analysis was: Zn, 6.17 pct; Mg, 2.13 pct; CU, 0.03 pct; Si, 0.009 pct; Fe, 0.005 pct; and the remainder, aluminum. An ingot -in. thick was cast, homogenized, hot and cold-rolled to strip 0.064-in. thick for dilato-metric and powder work, and to foil 0.005-in. thick for single crystal work. Solution treatment temperature for all specimens was 475°±5°C for periods of at least 1 hr, either in air furnaces or lead baths. Aging was done in oil or Pb-Bi baths controlled to within ±3°C. The aging was investigated at the following temperatures: room (30°), 130°, ZOO0, 260°, and 300°C. For the dilatometric study, the length changes were measured continuously, at temperature, using strips of alloy 10 in. long, shaped as channels to eliminate undesirable deflection due to bending. To compensate for thermal expansion and contraction due to the variations in the temperature of the aging baths, the dilatometers were built of the same alloy as the one being tested, with the same shape and size, but with material fully annealed. Gages on which 0.0005 in. could be read and 0.0001 in. estimated were used to measure the dilation. Length changes were also measured at room temperature. Strips approximately 10 in. long were solution-treated, quenched, and measured in a supermicrome-ter in which 0.0001 in. could be read and 0.00001 in. estimated. The specimens were immediately aged for a given time, remeasured, and then the cycle was repeated, including the solution treatment. The error of measurement with this technique was somewhat larger, but the results confirmed those obtained by continuous measurements. The sheet used for the dilatometric work was checked to determine grain orientation. Both X-rays and etching methods revealed a rather coarse grain size but only a negligible amount of preferred orientation. Thus, volume changes calculated from length changes are not invalidated by preferential orientation effects. Pieces of the sheet used for the dilatometric work were also used for the metal -lographic work. Filings for the powder X-ray study were produced from a homogenized piece of sheet. These filings were magnetically purged of iron, screened to 200 mesh, sealed in a Pyrex tube containing an argon atmosphere, and solution-treated. When quenching, the glass tube was broken, so that the powder dropped directly into cold water. After drying with alcohol, the powder was sealed into capillary tubes containing an argon atmosphere and then aged for the required times. In spite of all these precautions the three strongest lines of a( Al2o) appeared in all patterns, and were used as internal standards. By the use of these standards, accurate corrections for film shrinkage were obtained. For the back reflection patterns, annealed nickel powder was mixed with the specimen to act as internal standard. A preliminary investigation was made in small (57.3 mm diam) powder cameras. From these patterns the changes which took place in the solid-

Jan 1, 1957

By P. W. Neurath

IN recent years the domain theory of ferromag-netism has been put on a sound experimental and theoretical basis. But its application to one of the most widely used high quality magnetic materials, the cold-rolled grain-oriented 3 pct Si-Fe used in transformer cores, has been rather difficult because of the complexity of the domain structure of the poly crystalline sheet material. This paper presents some experimental data for this material, showing the relation between plastic and elastic stresses, 60-cycle watt losses, and the domain structure as observed visually. Only a very tentative qualitative explanation of the effects will be attempted. Some initial results were reported earlier.&apos;

Jan 1, 1957

By Joseph J. Yancik, Leonard L. Felts, George B. Clark

LITTLE information has been published concerning the actual or useful amount of energy obtained from explosives when they are used for blasting. To provide more data on this subject, 8-in. neet cement cubes were blasted in a steel plate box and the breakage energy evaluated by comparison with drop crusher results using Rittinger&apos;s,1,2 Kick&apos;s: and Bond&apos;s&apos; theories. Theories by Bond and Wang," Lineau," Hatch,&apos; Roller,&apos; and others0-11 were not considered applicable. Those used in this investigation may be expressed mathematically as follows: Rittinger Theory E = KrS2, pet,—--------------- [1] 40 d1 d0 Kick Theory TV 1 1 E = =K, [S pct. log1/d+ 100 log d0] [2] 40 d1 L. L. FELTS, Junior Member AIME, was formerly a Graduate Assistant, University of Illinois. G. B. CLARK, Member AIME, was formerly Professor of Mining Engineering, University of Illinois, and is now Chairman, Dept. of Mining Engineering, Missouri School of Mines and Metallurgy. J. YANCIK, Junior Member AIME, is a Graduate Assistant, Missouri School of Mines and Metallurgy. This paper, TP 4213A. is revised from a thesis submitted by L. L. Felts in partial fulfillment of the M.S. degree in Mining Engineering, University of Illinois, 1954. Discussion may be sent (2 copies) to AIME before May 31, 1956. Manuscript, Dec. 27, 1954. Bond&apos;s Third Theory E = Kb [S pct. log1/d1+ 100 log d0] where E — energy used in breakage, d, = average diameters of screen fractions of broken cement particles, pct, = percent weight of diameter d;, and 2 pct, = 100 pct. The above equations were employed to determine values of Kr, Kk, Kb for particle size distributions similar to those obtained from the blasting curves. These values were in turn used as a means of approximating the specific energy of the blasted material. The efficiency of crushing by blasting was then determined by dividing this specific energy by the maximum available work of the explosive per gram of cement. Knowledge of the failure of solids under static loads is developing very rapidly. Their failure under impact loads has been investigated and reported in the literature only to a limited extent. Theories of failure&apos; hnder static loading include 1) the maximum stress theory, 2) the maximum strain theory, 3) the theory of constant elastic strain, 4) theory of maximum shearing stress, and 5) Mohr&apos;s theory of strength. All of these have elements of usefulness in establishing an applicable theory for blasting. For highly strained and compressed material such as that surrounding a detonating charge of high explosive, the Mohr theory and its implications appear to be the

Jan 1, 1957

By V. A. Nieberlein

An extractive process was developed applicable to submarginal titanium deposits containing valuable minor constituents; such as columbium (niobium) and iron. The process consisted of reducing the mineral concentrate with coke at high temperature to form a carbide-suboxide sinter, chlorination in the 400° -500° C. range, and fractional condensation of the chlorides. The chlorination procedure recovered 97, 83, and 87 percent of the titanium from brookite, rutile, and ilmenite sinters, respectively, while simultaneous columbium recoveries on the same materials were 85, 50, and 87 percent.

Jan 1, 1957

By L. L. Mohier

Mr. Vissac&apos;s study is very elaborate and complete and gives a clear idea both of phenomena occurring during operation of the feldspar jigs and results ob- tained by some of them in Europe. I have no intention of going into a complete discussion, but I would like to give a few comments about these results already

Jan 1, 1957