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On Feb. 16, 1948, the Board of Directors of NME authorized the publishing of "Technical Notes" in METALS TECHNOLOGY. The purpose is to provide prompt publication of very short items of the following general types: I. Results of short investigations which do not warrant a paper. 2. The conclusions of extensive investigations of insufficient general interest to justify a regular paper. 3. Conclusions arising in the course of an investigation, which, because of interest to others in the field, the author wishes to present prior to completion of the investigation. 4. Pertinent factual comment (not mere argument) on the subject matter of previous "Notes." Such Notes will be subject to the approval of the Auxiliary and AIME Publications Committees, but can be handled more promptly than regular papers because they need not be referred to readers. The recommended maxi- mum length is 500 words; notes in excess of 1,000 words will not be considered for this type of publication. A graph or photograph may be included as part of the note when particularly illustrative. As with regular papers, contributions to the new section should be submitted to the Secretary of the AIME. Please furnish two copies each complete with illustrations.

Jan 1, 1948

On Feb. 16, 1948, the Board of Directors of AIME authorized the publishing of "Technical Notes" in METALS TECHNOLOGY. The purpose is to provide prompt publication of very short items of the following general types: I. Results of short investigations which do not warrant a paper. 2. The conclusions of extensive investigations of insufficient general interest to justify a regular paper. 3. Conclusions arising in the course of an investigation, which, because of interest to others in the field, the author wishes to present prior to completion of the investigation. 4. Pertinent factual comment (not mere argument) on the subject matter of previous "Notes." Such Notes will be subject to the approval of the Auxiliary and AIME Publications Committees, but can be handled more promptly than regular papers because they need not be referred to readers. The recommended maxi- mum length is 500 words; notes in excess of 1,000 words will not be considered for this type of publication. A graph or photograph may be included as part of the note when particularly illustrative. As with regular papers, contributions to the new section should be submitted to the Secretary of the AIME. Please furnish two copies each complete with illustrations.

Jan 1, 1948

By K. K. Kershner, W. A. Calhoun, C. W. Funk

Future resources of aluminum may require the utilization of low grade ores to provide a more permanent protection for the nation. Aluminum minerals such as cloy, shale, and high iron laterites may become important sources. An evaluation of reserves is given. New laboratory results are reported on the Vereinigte desilication process. THIS report on future resources of aluminum metal emphasizes the necessity for investigating utilization of low grade potential ores to provide more permanent protection for the nation. Partial or complete interruption of the importation of high grade aluminum ores must be given consideration. Ultimately, aluminum minerals such as clay, shale, and high iron laterites may become the principal sources of aluminum. The development of extractive processes for treating these low grade materials is a step in long-range national preparedness that should receive more attention. In formulating such processes, the application of beneficiation methods for the purpose of classifying the several types of minerals before subjecting each type to the more expensive extractive procedures should be considered, and a careful survey of the basic factors of power sources, transportation facilities, and sources of raw material should be made. Domestic Bauxite Resources Of the domestic supply of current, treatable-grade bauxite, 95 pct comes from Arkansas. The present reserve of Arkansas bauxite suitable for metal production, including abrasive-grade, Bayer-grade, and modified Bayer-grade ores, is 34,000,000 tons. The total reserve of bauxite of all grades is approximately 75,000,000 tons. Reserves are estimated on a mined and dried basis. Data available to the Bureau of Mines in 1948 to 1949 were used in preparing Table I, which shows a breakdown by grades of bauxite for about a half of the reserves of the state. The modified Bayer ore, 10,555,500 long dry tons, is based on a cutoff of 8 to 15 pct silica. The sub- marginal 10,074,700 long dry tons is assumed to contain more than 40 pct gibbsite, more than 15 pct silica, and less than 32 pct available alumina. A considerable amount of this low grade material was consumed in 1949 and 1950. Additional tonnages of bauxitic and kaolinitic clays are indicated by the Bureau of Mines drilling project.' Applying a 50 pct factor to arrive at long tons mined and dried, the results of this project are approximately 31,500,000 tons kaolinitic clay at +35 pct Al²O3 and 11,800,000 tons kaolinitic clay at 20 to 35 pct A1,0,. Total reserves of kaolinitic clays are probably quite extensive—several times the reserves shown in the Bureau's work. Total reserves of bauxitic and high iron clays from the drilling program and previously established figures are 63,980,000 tons. The mineral dressing methods,' the lime-sinter process, he lime-sinter modification of the Pederson process," the lime-soda sinter process,"-' and the Alcoa combination processa. have been described in the literature and will not be elaborated upon here. The less familiar Vereinigte Aluminium-Werke process used by the Germans during World War 11 may require some amplification. It was used to bene-ficiate boehmite ores containing 12 to 18 pct silica for a feed to the European Bayer process. Ore was

Jan 1, 1952

By Joseph J. Becker

RECENTLY the "oriented growth" hypothesis of recrystallization textures has been receiving considerable attention. According to this view, "whenever a new generation of grains is growing in a highly oriented matrix . . . one may assume . . . that from among available nuclei of a great variety of orientations those with suitable orientation relationship with respect to the matrix have by far the highest rate of growth (oriented growth) and will, therefore, predominate."' This statement includes primary recrystallization of single crystals and of polycrystalline materials showing strong deformation textures as particular cases. While the phenomenon of oriented growth undoubtedly does operate, and may be of importance in coarsening or secondary recrystallization, the writer feels that its extension to primary recrystallization is a different matter. Several aspects of this phenomenon may be pointed out which are difficult to rationalize on the basis of oriented growth. In recrystallizing deformed single crystals of alpha brass, Maddin, Mathewson, and Hibbard2 found that the twin composition planes of the recrystallized grains were parallel to the three operative slip planes they observed, and not to the fourth octahedral plane. The writer's current work seems to indicate further that when only one or two slip systems can be seen to operate, the recrystallized grains are aligned only with those slip planes actually observed. This behavior could hardly be accounted for by oriented growth, because on the latter basis the recrystallized texture of a deformed single crystal should certainly have the same symmetry as the crystal itself. Growth rates could not be expected to distinguish between crystallogra- phically equivalent directions, unless the presence of a visible slip system vastly increases the growth rate in the appropriate direction. This seems unlikely. These relationships were observed by the writer only when considerable care had been exercised before annealing to etch away the effects of cutting out the centers of tensile specimens with a jeweler's saw and to etch off the ends of compression specimens. When these.precautions were not taken, nu-cleation inevitably appeared to occur at the saw cuts or at the ends, and the resulting orientations never showed a [111] rotation but appeared quite random. The provision of many nuclei of many orientations did not enhance the correlation, but destroyed it. Recrystallization textures are sometimes strongly dependent on annealing temperature, which would imply that the anisotropy of growth rates is a suddenly varying function of temperature. This might be regarded as unlikely. Recrystallization textures can be strongly dependent on the degree of deformation. If textures are to be explained by selective growth from among nuclei of all orientations, it is difficult to see how the recrystallization process could have any dependence whatever on the manner or degree of deformation. It is felt that the above points should be considered before the oriented growth hypothesis is applied to primary recrystallization, with the necessary complete divorce of the mechanism of recrystallization from the details of the deformation process. References 1P. A. Beck and H. Hu: Reply to discussion of their paper on Recrystallization Texture and Coarsening Texture in High Purity Aluminum. Trans. AIME, 188, 1057; Journal oF Metals (Aug. 1950) TP 29083. 'R. Maddin, C. H. Mathewson, and W. R. Hibbard, Jr.: The Origin of Annealing Twins in Brass. Trans. AIME, 185, 655; Journal of Metals (Sept. 1949) TP 26763.

Jan 1, 1952

By J. S. Ll. Leach, J. B. Cohen, M. B. Bever

IN the work reported here, the heats of formation of a copper-rich Cu-Sn (a) solid solution and of the Cu.Sn (0 phase were measured by tin solution calorimetry. An approximate determination of the heat effect attending the precipitation of 6 from a supersaturated a solid solution was also made.

Jan 1, 1955

By David B. Burrows, Francis R. Conley

INTRODUCTION A prerequisite to the evaluation and management of oil properties is accurate information derived from the analysis of core samples; but reliable data, such as porosity and permeability, can result only if all oil and water have been removed from the core samples analyzed. The most common method of core cleaning used to date has been Soxhlet extraction—a somewhat static technique, which depends upon the slow diffusion of hot solvent through the core sample. Soxhlet extraction performs satisfactorily only with highly permeable samples and at best requires long cleaning periods. The centrifuge method was developed in 1951 by Continental Oil Co. to overcome the inefficiencies inherent in the Soxhlet method. The new method is basically an operation in which hot solvents are caused to flow through the samples under the influence of centrifugal force. The centrifuge unit has proved so successful that samples which formerly required days for partial extraction can now be completely cleaned in approximately one hour. The original idea was conceived in 1950 by Elmer S. Messer, whose early experiments consisted of flowing solvent over sandstone samples suspended in a revolving basket and driven by a vertically mounted vacuum cleaner motor. Results were so outstanding that more permanent units were constructed. A modified model using this basic design was recently built by Core Laboratories, Inc., and is now used regularly in their operations. DESIGN Fig. 1 shows a photograph of the two extractors routinely used to clean small core plugs in the Production Research Div. of Continental Oil Co.'s Ponca City laboratories. For illustrative purposes, the basket from one of the units has been removed, and because both extrac- tors are of identical design only one is described in the following discussion. Each extractor unit consists of a centrifuge and a solvent still. The core basket of the centrifuge is made of mild cold rolled steel 7 1/2 in. in diameter and 1 1/8 in. deep. The basket holds 18 1-in. samples (cubical or cylindrical) and is attached directly to a cone fitted to the shaft of the motor. Both the outer rim and the hollow hub of the basket contain perforations for the passage of solvent and extract. The solvent is delivered to the perforations by means of a copper tube inserted into the hollow hub. The motor is a vertical tool post grinder motor; (115 v, 5.6 amp, 0-60 cycles, AC-DC, rated at 1/3 hp). It has a rated speed of 10,000 rpm under full load and 15,000 rpm with no load. Variation of speed is obtained by the use of a variable transformer. The solvent still was constructed from one end of a stainless steel oxygen bottle by inserting a heating element, sight glass, and piping as shown on the schematic diagram, Fig. 2. The heater used was a three-position, 1,000 w, 115-v, immersion type. Intermittent flow of solvent to the centrifuge is obtained by means of a siphon bottle inserted between the condenser and the centrifuge.

Jan 1, 1957

By W. J. Carlson, I. Iwasaki

A previous article reported a combination process for recovering both metallic iron and metallic manganese from the manganiferous iron ores of the Cuyuna Range in Minnesota.' In this process, the iron was recovered by direct reduction and magnetic separation and the manganese was recovered from the nonmagnetic tailing by leaching and electrolysis. The current efficiency during the electrolysis of manganese is quite low, in the range of 60 to 70%, due to the simultaneous plating of hydrogen.2,3 The parameters that affect the current efficiency are (1) the concentrations of the manganese ion and the ammonium sulfate buffer, (2) the effect of autoxidant, (3) temperature, (4) pH, and (5) current density. To study the plating characteristics of manganese metal.

Jan 1, 1969

By M. T. Simnad, C. E. Birchenall, M. H. Davies

THE marker movements observed by Davies, Simnad, and Birchenall during the growth of magnetite on wustite have been misinterpreted. It is the purpose of this note to correct the original interpretation. In that investigation wustite specimens were prepared by oxidizing pure iron disks in water vapor until the iron was consumed. Argon was used as a carrier gas for the water vapor and on the complete conversion of the metal to its oxides ('FeO' plus a small amount (10 pct) of surface Fe3O) the water supply was bypassed and the specimens were annealed in argon alone in order to equilibrate the wustite with the overlying magnetite. After cooling, the magnetite was ground off, a crude magnetic test being employed to determine its complete removal. Radioactive silver streaks were then applied to the surface and the specimen was oxidized completely in water vapor to prevent hematite formation. After complete oxidation the markers were found to enclose about 80 pct of the magnetite with the other 20 pct lying outside the markers. This observation was interpreted to mean that oxygen transport was four times as great as iron transport during the growth of the magnetite. The conclusion would have been correct if, as in the case of wustite growing on iron, all the iron had started from one side of the marker and all the oxygen from the other side initially. Actually a material balance is required. For simplicity, take wustite to be exactly FeO, and magnetite to be Fe3O,. Then at the start of the reaction 3 FeO + O -> Fe,O., All of the iron and three-fourths of the oxygen of the final product will be within the marker inter- faces. The other fourth of the oxygen is in the gas phase outside the marker. From the experimentally determined final position of the markers simple calculation shows that one-fifth of the total iron has crossed the marker interface, while one-twentieth of the total oxygen has crossed in the reverse direction. The simplified result favors iron transport in the ratio four to one. However wiistite is not stoichiometric FeO. At 900°C, the temperature of the measurement, the composition is about FeO When the material balance for the same experimental result is repeated, assuming the product will be 1 mol of Fe3O4, it is found that 0.6 gram atoms of iron and 0.19 gram atoms of oxygen must have passed the marker in the same direction. (This is readily apparent from the reaction to form 1 mol of Fe3O4 SFeO The total oxygen supplied from the atmosphere is 0.61 gram atoms, but the iron which passes the marker interface, i.e., 0.6 gram atoms, requires 0.8 gram atoms of oxygen to convert it to Fe,O,.) If all the transport during magnetite growth is due to iron ion diffusion, then the marker would enclose about 85 pct of the final magnetite and the original measurement is in error by about 5 pct. This error is probably less than the uncertainty in locating the markers by autoradiography. The possibility also exists that the starting wustite was not quite saturated with oxygen and underwent further enrichment with consequent envelopment of the marker before magnetite caught up with the marker interface. In any case it appears that these measurements actually favor iron ion diffusion in magnetite overwhelmingly as the factor controlling its growth, although further experimental measurements are needed to eliminate the error in material balance described. Such studies are planned.

Jan 1, 1954

By P. Greenfield, P. A. Beck

RECENT work by J. Darby, Jr. in this laboratory has shown that the reported vanadium-rich limit of the s phase in the Co-V system at 1200°C is in error. The appearance of a second phase in s actually is restricted to alloys containing over 68 atomic pct V. The error in the original value is due apparently to a reaction that takes place along the numerous cracks in the s specimens between the alloy and the impurities present in the He + 8 pct H atmosphere in the annealing furnace. Such a reaction and the consequent appearance of a second phase can be suppressed if the alloys are sealed under vacuum in Vycor tubing. The new value of 68 atomic pct V for the vana-dium-rich limit of the s phase in the Co-V system effects slightly the s compositions calculated from average values of N, and N,. for various s phases. The standard deviation between experimental mean compositions and those calculated from the assumption that s is characterized by a constant number of 3d + 4s electrons per atom (N,), is slightly reduced from 9.1 to 8.8 pct. The maximum divergence for the V-Mn s phase is reduced from 15.5 to 14 atomic pct. The standard deviation calculated from constant electron vacancy numbers given by N.. = 4.66 (Mo + Cr + V) + 3.2 (Mn) + 2.2(Fe) + 1.71(Co) + 1.6(Ni) is now greatly reduced, as the maximum divergence for this correlation previously occurred in the V-Co system. This maximum divergence is reduced from 7.6 to 2.3 pct, and the standard deviation for all s- phases is reduced from 4.1 to only 2.9 pct. The correlation for electron vacancy numbers given by N. 5.66 (V when with Ni or Co) + 4.88 (V when with Mn or Fe) + 4.66 (Cr + Mn) + 3.3 (Mn) + 2.66 (Fe) + 1.71 (Co) + 0.61 (Ni) is made slightly worse, and the standard deviation increases from 2.8 to 3.9 pct. These changes, however, do not affect the conclusions of the paper.' The deviation between calculated and experimental s compositions is much less for either one of the electron vacancy correlations than for the correlation with the number of 3d + 4s electrons.

Jan 1, 1955

By A. J. Opinsky

MANY investigators, in their discussions, have reasoned that the ductile-brittle transition in iron could be explained by the intrusion of cleavage into the normal slip process. The purpose of this note is to apply the laws of critical normal stress for cleavage and critical shear stress for slip to explain the orientation and temperature dependence of the ductile-brittle transition in body-centered cubic metals. It will be found that within a certain temperature range, single crystals tested in tension will cleave or slip, depending on their orientation. Some data recently appearing in the literature will be analyzed from this standpoint. For a single crystal with [uvw] parallel to the tensile axis, the resolved shear stress on the slip

Jan 1, 1954

By J. L. Huitt

Some of the problems associated with the acid treatment of oil wells are related to the control of the composition of formation treating acid. One test usually made at the well site is the determination of the acid concentration. Heretofore, the concentration of the acid delivered to the well site usually has been interpreted from a hydrometer measurement of the specific gravity of the acid solution. Experience has shown that this indirect measurement of acid concentration can give erroneous results. More reliable results are, of course, obtainable by the titration method; however, this method is not easily adapted to well-site testing. To overcome these objections, a device was developed for use in the field which permits determination of the concentration of treating acid both quickly and accurately at the time of the acid treatment. Its purpose was three-fold, namely, to determine: (1) the concentration of the fresh treating acid, (2) the concentration of the spent acid returning from the well, and (3) the solubility of formation samples in treating acid. The device was designed to operate on the principle of the stoichiometric relation between the calcium carbonate—hydrochloric acid reaction and the carbon dioxide gas resulting from the reaction. By confining the carbon dioxide gas within a reaction cell of the type shown in Fig. 1, the pressure inside the cell is increased. Since the pressure is an indication of the quantity of carbon dioxide gas produced, it may be used to estimate the concentration of the acid, provided an excess of calcium carbonate is used. From information on the volume of the reaction cell, the volume of acid used, and the pressure and temperature of the gas after the completion of the reaction, the concentration of the treating acid may be computed. The reaction cell is essentially a pressure vessel equipped with a pressure gage, temperature indicator. pressure release valve, and a special sample holder. Plastic and metal construction makes the cell both rugged and acid-resistant. The sample holder is so designed that a sample of calcium carbonate (or sample of carbonate rock) can be dropped into the acid

Jan 1, 1956

By H. L. Sauder, J. L. Newman, C. Waddell

An instrument capable of measuring subsurface flow rates is described. The instrument is self-contained and may be run on piano wire line. It detects flow by means of an impeller suspended between two torsion wires. The force of the well fluid striking the impeller causes the impeller to rotate, exerting a torsional force to the wires. This force is determined by recording the angle of rotation of the impeller on film using a battery-driven, clock-controlled camera. The impeller is sensitive to flow in either direction and the same instrument can be used to measure injection as well as production rates. Changes in direction of flow, such as might be caused by thief zones, are measurable and are indicated by a reversal of the direction of rotation of the impeller. Adjustment of the sensitivity of the instrument to measure a wide range of flow rates is accomplished by the use of different size torsion wires. An umbrella-type fluid trap, which contacts the casing or wellbore, diverts the flow through the flow tube. The fluid trap remains closed while rurrning in the hole and can be opened at any point in the well. The instrument with the trap closed is 1 3/4 in. OD and may be run through 2 in. tubing. Successful flow profiles have been made on wells with flow rates ranging from 60 BID to 4,000 B/D at surface pressure up to 4,500 psi. The instrument is designed for high-pressure and high-temperature operations. INTRODUCTION The need for an instrument that will measure flow rates in a wellbore is as old as reservoir engineering itself. A number of such devices have been designed within the past few years. Some of these have been described in the literature1,2,3,4,5,6 One of these devices1. a hot-wire anemometer type, made many successful jobs in dry gas producing areas. Difficulty was encountered when this flowmeter was used in wells producing liquids and development work was initiated to overcome this difficulty. The present flowmeter is the result of this work and provides an instrument with a wider range of application in the industry. Consider- able development work has been done on the tool involving many changes in the mechanics of recording the flow readings, however, the basic principle of flow detection has remained the same since its inception. PRINCIPLE OF OPERATION The basic principle of operation of the flowmeter is the utilization of a portion of the kinetic energy of flowing well fluid to impart a rotational force to an impeller suspended between two torsion wires. This impeller, Fig. 1, is a screw-type propeller with the blades having a pitch angle of 40. As the well fluid passes through the instrument it strikes the impeller. The resulting force rotates the impeller and twist\ the torsion wires to a balance point at which the torque imparted to the wires balances the force required for the impeller to deflect the well fluid. The impeller is symmetrical and a change in direction of the flow results in a reversal of the direction in which the impeller is deflected. Thus the direction of the flow as well as its velocity is indicated. A dial is attached to the impeller by means of a hollow tube through which the upper torsion wire extends. The angular position of the impeller is recorded by photographing the dial at frequent intervals. In any given set of torsion wires the modulus of shear and polar moment of inertia remain constant and the deflection varies directly with the applied torque. The deflection imparted to the torsion wires also varies as the square of the fluid velocity. Further, the velocities represented by any two given deflections hear the following relationships: and Where V = velocity of flow stream and O ;= deflection. This is the basic relationship which is used to calculate the relative velocities represented by a given set of deflections where the velocity represented by any one of the deflection readings is a known quantity. For a given torque, the deflection of the torsion wire varies inversely as the fourth power of the wire diameter. Wire sizes ranging from ,005 in. in diameter to .022 in. in diameter can be used. The range of

Jan 1, 1957

By John R. Spencer

A capillary tube variable volume cell is described, which has operated satisfactorily over a range of 100°F and 3,500 psi to 550°F and 1,500 psi. The cell contents are entirely visible over the length of the capillary with the exception of a space at the top amounting to three per cent of the total volume. Observations on the critical behavior of simple systems have been greatly facilitated by the apparatus, it being possible to establish the critical conditions for a particular mixture in the course of a day's run. INTRODUCTION Many types of apparatus have been designed for obtaining data on the phase relationships of hydrocarbon systems. Such apparatus can in general be subdivided into two classifications; (l), indirect measurement of phase volume, and (2), direct visual observation of phase volume, each of which has outstanding advantages and disadvantages. Indirect measurement of phase volume requires the use of rather elaborate apparatus including internal probes in which are located the device for determining the locus of the interface between phases. Such equipment is by its very nature costly, and is complex from the standpoint of operating technique. Probing techniques can be used, however, over wide ranges of temperature and pressure with a high degree of reproducibility. Apparatus for visual observation of phase behavior obviously has the advantage of enabling the experimenter to see exactly what takes place, but because the material to be tested is contained in a cell constructed of both metal and glass, is limited severely as to the temperature range of operation. Furthermore. the maximum pressure usually is limited by the choice of material used for sealing the glass to the metal, and by the strength of the glass itself. In the interest of increased efficiency of observation, as much of the cell as possible should be visible to the eye. Glass capillary tubes have been used successfully but have always given difficulty at the metal-to-glass seal. An apparatus has been devised to overcome the problems of sealing and resistance to temperature effects that have heretofore been the limiting factor with glass apparatus in the observation of phase volumes at elevated temperature and pressure. APPARATUS The objective which dictated the general arrangement of the apparatus (Figs. 1 and 2) was simplicity of operation. The air bath, A, was constructed of an iron framework to which was attached approximately one inch of glass wool bats which were covered on the outside with "Masonite." A roughly octagonal center piece was installed to provide forced circulation of the air by the fan, B, past the heaters, D, cell, F, and thermoregulator, C, respectively. The entire top of the box is removable to facilitate charging of the cell and to permit easy maintenance. Two windows are provided before and behind the cell to allow the operator to observe the contents against the background fluorescent light, E. The heaters,

Jan 1, 1951

By John R. Spencer

A capillary tube variable volume cell is described, which has operated satisfactorily over a range of 100°F and 3,500 psi to 550°F and 1,500 psi. The cell contents are entirely visible over the length of the capillary with the exception of a space at the top amounting to three per cent of the total volume. Observations on the critical behavior of simple systems have been greatly facilitated by the apparatus, it being possible to establish the critical conditions for a particular mixture in the course of a day's run. INTRODUCTION Many types of apparatus have been designed for obtaining data on the phase relationships of hydrocarbon systems. Such apparatus can in general be subdivided into two classifications; (l), indirect measurement of phase volume, and (2), direct visual observation of phase volume, each of which has outstanding advantages and disadvantages. Indirect measurement of phase volume requires the use of rather elaborate apparatus including internal probes in which are located the device for determining the locus of the interface between phases. Such equipment is by its very nature costly, and is complex from the standpoint of operating technique. Probing techniques can be used, however, over wide ranges of temperature and pressure with a high degree of reproducibility. Apparatus for visual observation of phase behavior obviously has the advantage of enabling the experimenter to see exactly what takes place, but because the material to be tested is contained in a cell constructed of both metal and glass, is limited severely as to the temperature range of operation. Furthermore. the maximum pressure usually is limited by the choice of material used for sealing the glass to the metal, and by the strength of the glass itself. In the interest of increased efficiency of observation, as much of the cell as possible should be visible to the eye. Glass capillary tubes have been used successfully but have always given difficulty at the metal-to-glass seal. An apparatus has been devised to overcome the problems of sealing and resistance to temperature effects that have heretofore been the limiting factor with glass apparatus in the observation of phase volumes at elevated temperature and pressure. APPARATUS The objective which dictated the general arrangement of the apparatus (Figs. 1 and 2) was simplicity of operation. The air bath, A, was constructed of an iron framework to which was attached approximately one inch of glass wool bats which were covered on the outside with "Masonite." A roughly octagonal center piece was installed to provide forced circulation of the air by the fan, B, past the heaters, D, cell, F, and thermoregulator, C, respectively. The entire top of the box is removable to facilitate charging of the cell and to permit easy maintenance. Two windows are provided before and behind the cell to allow the operator to observe the contents against the background fluorescent light, E. The heaters,

Jan 1, 1951

By C. C. Harris

The Gaudin-Meloyl equation for the size distribution of fragments resulting from single fracture is where y is the mass fraction of material smaller than size x, and x, and r are parameters to be determined from the experimental data. In physical terms, r is associated with the number of active flaws in a particle of characteristic dimension xo . The special attribute of this equation is its emphasis on the coarse size region of a distribution. There are various procedures2-5 for obtaining the parameters in Eq. 1, but a simple graphical method is awaited. This situation contrasts sharply with that in the cases of the familiar Gates-Gaudin-Schuhmann and Rosin-Rammler equations.6 The purpose of this note is to present a method based on a procedure7 which has been successful in several other applications.8-13

Jan 1, 1967

By A. L. Simpson, J. M. Edwards

The application of the Scintillometer to radioactivrty surveys in boreholes of oil wells has made it possible to determine bed thickness with a high degree of accuracy. This fact, combined with known relation of logging variables, makes thin bed porosity determination practical. With the use of the Scintillometer a method hot been derived whereby the apparent level of radiactivity, as recorded on radiation logs, may be converted to the true level. The true level of radioactivity is that level to which the recording pen would have traveled had the detector remained at a given depth for on infinitely long period of time. This factor is: radioactivity level, Ra, is the apparent radioactivity level, T is the bed thickness, D is drag, and L is the length of the detecting system. This method depends entirely on accurate measurements of bed thickness and drag. A thorough discussion of the concept of time constant and logging speed as related to drag is undertaken. INTRODUCTION Neutron curve interpretation has become one of the accepted methods for porosity determination in oil field practices. A great deal of literature has been published about neutron derived porosities, but this has been concerned with thick beds, or possibly even averaging of a series of thin beds as a single unit. There has been a lack of written information on methods whereby porosity can be evaluated for beds less than 10 ft in thickness. In certain areas, production is derived from relatively thin formations. The importance of thin bed evaluation, the fact that the Scintillometer is an adequate tool for this application, and the general lack of published information concerning neutron porosity for thin beds are the fundamental reasons for presenting this method of porosity determination. This concept is not put forth with the idea of discounting existing methods, but is merely suggested as a modification of other accepted methods of porosity determination which makes no allowance for quantitative evaluation of thin beds. The effects on the neutron log of counting statistics, statistical variation in the porosity of earth materials, and hole size must be taken into account to obtain neutron derived porosities. Since these effects have been described in past literature, the authors have not made an attempt to go into the subject in detail. With the use of statistical and repeated sections on the log, it may be determined which responses on the log actually correspond with lithologic changes. EFFECT OF DRAG AND ITS RELATIONSHIP TO TIME CONSTANT AND LOGGING SPEED Before entering into a discussion of porosity determination of thin beds, there should be a thorough

Jan 1, 1956

By R. A. Deju, R. B. Bhappu

The theory of electrophoresis is briefly outlined and an apparatus which may be used for electrophoretic studies is explained. The results obtained using this apparatus are in agreement with those obtained by other investigators. How to solve some of the complications which occur in the measurement of zero charge and zeta potential is explained. It is believed that the apparatus described in this paper will allow rapid measurements of zeta potential, zero point of charge, electrophoretic mobility and zeta coefficient. For many years the phenomenon of electrophoresis has been studied, and much work has been done in designing an apparatus for better measurements of mobility, zeta potential and zero charge of minerals. Up to the present, most electrophoresis experiments have involved cumbersome equipment and tedious microscopic observation. The modified cell proposed in this paper obviates these drawbacks by using a Rayoscope together with a special system of lenses and filters. It therefore allows a faster and more accurate measurement of zero charge and particle velocity. THEORY Most authors currently regard zeta potential as the potential difference in an otherwise uniform medium between a point some large distance from the surface of the mineral and a point on the plane of shear. Fuerstenau,1 Miaw,2 and Gaudin and sun3 have performed some calculations of zeta potential using Henry's equation.4 Their results show wide discrepancies, probably due to differences in the past histories of the minerals used. The authors have also noticed this difference on determining the zero point of charge of quartz as shown on Table I.

Jan 1, 1967

By William L. Russell

A new instrument for measuring bulk and grain vol-urnes is described, and compared in accuracy with two modifications of Nutting's method, All three methods are reasonably fast, and in all three the probable error in the determinations of bulk volume can be kept down to about 0.1 to 0.2 per cent. INTRODUCTION The new pycnometer described in this paper is designed to give speed without sacrificing accuracy. Some time ago Russell1 described a somewhat similar appa-ratus; however, the instrument described in the present paper is more accurate. Nutting' designed the pycnom-eter shown in Fig. 1 (A and B), and Pirson3 has shown points like those of Fig. 1-D. The procedure described in this paper for using Nutting's pycnometer has been modified from that used by Nutting. CHOICE OF LIQUIDS The best liquids for measuring grain volumes are hydrocarbons or chlorinated hydrocarbons which evaporate slowly. Trimethylbenzene or mesitylene, triethylben-zene, carbon tetrachloride, and tertalin have been used for this purpose. Any of these liquids or mercury may be used for measuring bulk volume. PREVENTING ERRORS DUE TO INVASION OF LIQUID Errors due to the invasion of the porous, permeable bulk samples by the liquid of measurement may be prevented or greatly reduced by using mercury, by applying an impervious coating, or by soaking the bulk samples in the liquid of measurement until bubbles cease issuing from them. Errors are produced only by the invasion of the samples which occurs between movement when the samples are weighed in air and the moment the weight of liquid displaced by the sample in the pycnometer is determined. No error is produced by varying degrees of filling of the pore space of the samples by the liquid of measurement. The excess liquid should be wiped from the samples immediately before the weight in air W1, is determined, and they should be placed in the pycnometers immediately. OPERATION OF NEW INSTRUMENT The new pycnometer is shown in Fig. 2. It consists of two glass parts which fit together at a ground glass joint. The spaces J and D are connected by fine glass tubes E, and the space J must be larger than the space D by at least the volume of the largest sample to be tested. The projections H afford a grip for twisting when the two parts tend to stick together. The position of the sample in mercury is shown by I, and in other liquids by M. F is a permanent mark on the glass, and G is a tem-Some marker. In order to determine the position at which G should be placed, invert the instrument so that A is at the bottom, and fill space D. Place the cub K

Jan 1, 1958

By George W. Crawford, W. P. Aycock, E. W. Hough

Forty oilfield brines have been examined so far by a polarographic technique new in petroleum engineering called the "tensatnmetric method" by the team of biochemists who perfected its use in their field. Samples of brine were obtained from various oil fields in which the wells were known to be producing fluid from oil productive zones in well-known geologic formations. Most of the reservoirs from which the samples were obtained are believed to have an active water drive under the prevailing conditions of operation. The 40 samples represent brines produced front 16 different formations of various geologic ages. Graphs have been prepared of the data obtained in the testing of each sample, and the distinctive waife-like curves so obtained are characterized by reproducible profiles, called "response curves." Careful comparison of the response curves of salt water coming from different fields producing from the same geologic formation reveals that the curves are similar. The response curves of salt water coming from productive zones of different geologic formations are characteristically different. Preliminary work offers the further hope that response curves of an oilfield brine indigenous to a particular oil-bearing formation and hence representative of a particular geologic environment, such as deposit-ional and all subsequent morphological conditions, may be of value in reservoir engineering in the interpretation of surface and interfacial phenomena. For example, the wettability of the rock matrix and more specifically, the classification of productive oil-bearing strata as hydrophyllic or hydrophobic may be determinable. However, many more brines must be examined and the resulting response curves analyzed in comparison to known causal phenornena before this objective is achieved. INTRODUCTION One of the perennial moot questions in the literature of petroleum engineering is whether the reservoir rock is oil- or water-wet. Possibly an answer to this question could come from a careful examination of oilfield brines. None of the conventional methods of examining brines (chemical analysis, pH and electrical conductivity measurements, and the like) answer the question. Careful analysis of reservoir behavior observed in the exploitation of oil fields, particularly in the application of fluid injection, has been fruitful to the extent that a few reservoirs are believed to be properly classified. Physical chemistry suggests the behavior of reservoir brine and rock may be due to something in the brine in small amount. The ever increasing development and modification of theory in the general field of surface and interfacial chemistry has, and is, contributing to a better understanding of the problem, particularly as theory is verified by data. The work herein reported was begun in 1953 by Hough and Roebuck 1,2 who employed a new form of alternating current polarography, i.e., tensammetry, developed by Breyer, et a13,4 and who studied eight oilfield brines in adapting tensammetry to petroleum engineering needs. THEORY AND DEFINITIONS Tensammetry is a new technique of inquiry into surface phenomena. Specifically, a weak alternating current voltage is superimposed upon the direct current voltage applied to a dropping mercury electrode in contact with an electrolyte containing a small amount of a surfactant. The resultant alternating current can be measured and provides the experimental data for this new area of research. Under the influence of the direct current voltage, polar molecules arrange themselves in a double layer at the electrode. This double layer may be compared to a variable condenser, the capacitance of which is a function of the imposed direct current voltage. The direct current voltage determines the degree of adsorption of the surface active molecule on the electrode. Whenever the molecules are strongly adsorbed on the electrode, the capacitance of the double layer is low and the alternating current through the cell is low. Desorption occurs at some values of the direct current voltage, and at these voltages the capacitance of the double layer is high, resulting in an increase in the alternating current through the cell. The direct current

Jan 1, 1958

By M. R. J. Wyllie, F. Morgan, P. F. Fulton

The importance of formation factor, F, not only in electric logging but as a fundamental rock parameter has recently been stressed.',: The desirability of investigating the range of variation of the resistivity index exponent, n, in the relationship I = S ;", where I is the resistivity index and Sw the water saturation as a fraction of the void volume of a porous medium, has also been urged.3 The magnitude and variation of n with saturation and rock texture is a subject not only of theoretical interest but also one of prime importance in the interpretation of electric logs. A simple technique has recently been developed which enables both F and u to he measured with high accuracy and which may also find acceptance as a convenient method for the determination of irreducible saturation attainment in the restored state method of core analysis. Experience has taught that reproducible measurements of F are possible only if the resistance measuring electrodes are so arranged with respect to a plane face on a porous medium that they are able to make electrical contact with substantially all entry pores in that plane. In practice this may be achieved by using a platinized-platinum gauze electrode backed by some absorbent material (such as felt) which has been saturated with a fluid identical with that used to saturate the porous medium. Applicatiorl of pressure to the electrode and absorbent material then forces the gauze against the plane face of the porous medium and simultaneously squeezes saline solution through the meshes of the gauze. By this means the electrode is in continuous aqueous contact with all pores and satisfactory and reproducible low resistance contact with the porous medium is achieved. Clearly this method, although satisfactory for measurements of F, cannot be applied to the making of continuous resistance measurements on a porous medium while capillary pressure desaturation is being carried out. However, accepting the principle that for satisfactory results electrical contact must be made between a measuring electrode and all pores adja- cent to that electrude, methods of bringing electrodes into intimate contact with the surfaces of porous media were investigated. Two methods were ultimately found to be satisfactory: in the one, the metal electrode is formed on the required portion of the porous medium by the use of a metal spray gun, while in the second the electrode is painted on with an ordinary camel's hair brush. The first method has the advantage of permitting the use of any metal which can be sprayed, but has the disadvantage of requiring rather elaborate and expensive equipment. The second method is presently limited to silver electrodes although in principle other metals, e.g. platinum or gold, could be used. Moreover, the method is so simple and cheap, and has been found to be so satisfactory that it will be described in some detail. The core being investigated is cut into a right circular cylinder and is extracted and dried in the usual manner. The ends are then lightly painted with silver conducting paint* of the type used in printed electrical circuits. The quantity of paint used is not critical but the recommended, minimum compatible with entirely coating the core ends is recommended, particularly on the end that contacts the barrier. The core is then dried at atmospheric temperature for one hour or for shorter periods at any suitable elevated temperature up to about 110°C. It will be found that silver coatings so prepared are not only strongly adherent but also permeable and the core may be the core may be desaturated by the ordinary capillary pressure technique through one of the coated faces. The same permeability is characteristic also of thin metal coatings formed using the spray-gun technique. An ordinary Lucite capillary pressure desaturation cell has been adapted to a form suitable for measuring the resistivity of the saturated silver faced cores both at 100 per cent saturation (i.e., F) and at intermediate saturations down to the irreducible minimum. This has been achieved as follows: A Coors porcelain barrier, having a displacement pressure of c 30 psi was grooved across a diameter. Dimensions of this groove were c 1 mm deep and 1 mm wide at the top. The groove was then painted thickly with silver conducting paint, the paint in the groove being extended lightly over the edges of the groove for a distance of c 1 mm on each side. A 30 gauge silver wire was then arranged in the groove in a form of a spring bow, each end of the silver being held at diamet~ically opposite ends of the groove by means of plastic cement. The arc of the bow at its highest point was arranged to be a millimeter or so above the face of the barrier, while one end of the bow wire was led by means of a pressure-tight connection through the wall of the capillary pressure cell. The groove in the barrier was then Surrounded by suitably cut portions of Kleenex in the conventional manner so as to ensure capillary continuity from core to barrier, and the core placed on the barrier. The weight of the core distorted the silver spring bow and good electrical contact was thereby made between the outside of the cell and the lower painted silver electrode. Electrical connection to tile top painted silver

Jan 1, 1951