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By Merlon C. Flemings, Theodoulos Z. Kattamis

Examination was made of the distribution of tnanganese and nickel in colutrrnar dendrites of a cast low-alloy steel; more limited work was corzducted on chromium. Corresponding "segregrction ratios" were calculnted and shown to be relntivelv insensitive to cooling rate (''segregation ratio" is defined (Is the ratio of maximum to minimum concentrations within a volume whose dimensions are the order of the dendrite-arm spacing). Isoconcentratiorl curves were determined by the electron micropvobe and by rt7etallografihic studies on specimens subjected to isothermal-transformation treatments. From construction of isoconcentration curves, morphology of columnar dendrites is descvibed as intermediate between Perfect rodlike and sheetlike morphologies. The study is extended to equiaxed dendrites and it is shown that the strcture of these dendrites is sittlilar in many respects to that of columnar dendrites. On the basis of tlze sheetlike morphology of dendrites, a simple model is pvoposed for calculation of honzogenization kinetics. Results of trzatllevlatical analysis brcsed on this utzodel are given. This analysis relates residual segregation to time at homogenization temperature; it is in agreement with experiment. Calculations are given which show that even for relatively rapidly cooled material (of 1-ine dendrite-artn spacing) treatmets at 1200°C or above are necessary to achieve slgxificant Izomogenization of elenlents other than carbon itz reasonable time (e.g., rnangclnese, nickel). Conlplete homogenization of carbon is obtnined at much lowev tenlperatures (below 870°C). IN dendritic solidification of castings and ingots, solute redistribution during freezing results in mi-crosegregation of most alloy elements. The micro-segregation is such that minimum solute concentrations occur at the center of dendrite arms and maximum concentrations occur between dendrite arms. Residual segregation after subsequent therma1 processing (homogenization) depends on maximum and minimum initial concentration, on the detailed geometry of the isoconcentration surfaces within interdendritic regions, on the diffusion coefficient of the solute, and on time of thermal processing. The objective of this work was to determine, for a low-alloy steel, maximum and minimum concentrations, and the geometry of isoconcentration surfaces, primarily in order to permit calculation of homogenization kinetics. Most of the work reported was conducted on Samples from a unidirectionally solidified, fully columnar ingot. This type of ingot is made by extracting heat during solidification from one face; techniques for accomplishing this have been discussed.' Samples were taken at several locations, up to 5.75 in. from the mold chill face; the bulk of the work was performed on samples at 5.75 in. Alloy cast was, nominally, 0.4 pct C, 1.8 pct Ni, 0.8 pct Cr, 0.7 pct Mn, 0.25 pct Mo, 0.3 pct Si, and the balance iron. Brief study was also made on samples from an ingot which solidified with equiaxed grain structure. SAMPLE PREPARATION AND ANALYSIS Samples for electron-microprobe analysis were incorporated in mounts that included pieces of electrolytic nickel, chromium, and manganese, in order to normalize the intensities of these solutes in the specimens; also, a piece of electrolytic iron was included to measure the background. All specimens were polished in the usual metallographic manner. After the microprobe traces were made, the path was revealed by etching the specimens with picral. All microprobe analyses were made by point counting, integrating for 30 sec. The distance between points was fixed from 2 to 10 p, according to the precision desired in each case, the fineness of the structure, and the concentration gradient existing in a given area. (The distance was chosen 2 to 5 p near the maximum-concentration regions and 5 to 10 p near the minimum concentration.) The "take-off" angle for the A.R.L.-Model No. 21000 microprobe employed was 52.5 deg. Samples for metallographic analysis of isoconcentration curves were prepared by austenitizing at 1540°F for 20 min, quenching to the nose of the TTT curves (1200°F), heat treating isothermally at this temperature for a given time 0, and then quenching to room temperature. Due to concentration gradients existing in a dendritic structure, no transformation will take place for a given time 0 of isothermal heat treatment in the regions where the a.lloy concentration is higher than a given limit. Thus, the dendrite appears limited by an isoconcentration curve and can be made to appear to grow by varying the time of isothermal heat treatment.

Jan 1, 1965

By G. R. Speich

The age-hardening of Fe-18 to 21 pct Ni marten-sites containing small amounts of titanium, aluminum, copper, or molybdenum has been studied by hardness measurements, transmission electron microscopy, extraction replicas, and X-ray and electron diffraction. Electyon-probe microanaly-sis of the extracted precipitates was also performed. The effects of temperature and composition on the aging kinetics have been studied in detail for Fe-20 pctNi-Ti martensites. All the martensites hardened on aging at 400" to 500 "C with a single aging peak. In the Fe-20 pct Ni-Ti martensites hardening was associated with the formation of a fine dispersion of NisTi. No precipitation was observed in an Fe-21 pct Ni-2.6 pct A1 alloy, although the hardness increased from 327 to 545 Dph during aging at 500°C. Copper was precgitated from an Fe-20 pct Ni-10.7pct Cu alloy, at least during the later stages of age-hardening. Hardening in an Fe-18 pctNi-5pct Mo alloy was associated with the precipitation of an intemzetallic compound tentatively identified as NisMo. The formation of austenite and the recovery of the defect structure of the martensite occur simultaneously with the normal precipitation processes &ring aging of these alloys. THE age-hardening of substitutional iron-base martensites is an important subject for study since age-hardening is one of the principal means of strengthening the substitutional iron-base martensites in precipitation-hardening stainless steels1 and maraging steels.a~4 In contrast to Fe-C martensites, these martensites are relatively soft and ductile in the as-quenched condition, due to the low solid-solution hardening effect of the substitutional elements as compared to carbon. Also, these martensites are hardened by aging at low temperatures in contrast to Fe-C martensites which generally soften on tempering. Titanium and aluminum, singly or in combination, as well as copper and molybdenum, have been the principal alloying additions to stainless steels to obtain an age-hardening reaction.' Ti-A1 or Co-Mo-Ti combinations have been used in the case of maraging steels.3"4 The present work has been confined to a study of the age-hardening characteristics of an Fe-18 to 21 pct Ni martensite to which small amounts of titanium, aluminum, copper, and molybdenum were added in order to study the effects of each alloying element separately. The age-hardening characteristics of these alloys were studied by hardness measurements, transmission electron microscopy, extraction replicas, and X-ray and electron diffraction. Electron-probe micro-analysis of the extracted precipitates was also performed. The types and dispersion of precipitates, the formation of austenite, and the recovery of the defect structure of the martensite all were studied. EXPERIMENTAL PROCEDURE Alloys. The compositions of the alloys studied are listed in Table I. The level of 18 to 21 pct Ni was chosen to assure complete transformation to martensite on quenching and is the same nickel level used in maraging steels. The concentrations of titanium, aluminum, copper, and molybdenum were chosen after a study of the and Fe-Ni-MO' ternary diagrams indicated how much of each alloying element could be dissolved in austenite. Alloys with 2 and 4 pct Cu were also studied, but these did not show precipitation hardening at the nickel levels studied and will not be discussed further. The alloys were prepared from electrolytic iron and high-purity* nickel, titanium, aluminum, copper, and molybdenum by vacuum melting of 20-lb heats. These were vacuum-cast into two 8-lb ingots. The ingots were hot-rolled at 1100°C to 1/2-in. plate and subsequently cut into 3/8-in. cubes. The cubes were sealed in evacuated quartz capsules and solution-treated for 16 hr at 1100°C, except for the Fe-20 pct Ni-10.7 pct Cu alloy and Fe-21 pct Ni-2.6 pct A1 alloys which were solution-treated for 16 hr at 1300" and at 1250"C, respectively. Metallographic examina-

Jan 1, 1963

By Nicholas J. Grant, A. W. Mullendore

Measurements of grain boundary sliding were made on polycrystal and bicrystal tensile creep specimens of Al-2 pct Mg at 500oand 700oF. Grain and pain boundary orientation factors were studied with respect to their effect on the magnitude and direction of grain boundary sliding. It was concluded that a large part of the observed sliding may be caused by the operation of slip crossing the grain boundaries. Supporting evidence for this model from other investigations is also given. GRAIN boundary sliding in metals during elevated temperature deformation has frequently been thought of as an independent mechanism with its own characteristic stress, temperature, and structure dependence. Further, it is common to regard the grain boundary as the weak link during creep deformation since: 1) the strength of apolycrystallinemetal, as meas-sured by creep rate or rupture life, decreases at\a more rapid rate when sliding comes into action, and 2) grain boundary sliding, as revealed by "boundary darkening" and fold formation is often the first visible deformation. On the other hand, more quantitative observations, in both polycrystals and bicrystals, have shown boundary deformation to be closely related to the over-all deformation of the specimen. The curve of grain boundary contribution to elongation vs time takes a shape similar to that of the total creep curve,',' and the apparent activation energy for sliding appears in most cases to have the same value as that for total creep.3 In order to reconcile these observations, one is left with these possibilities: 1) The grain boundary and grain deformation rates are both controlled by the same rate limiting processes. 2) The rate of sliding is limited by accommodation deformation in the grains. 3) Sliding is the consequence of grain deformation. 4) Grain deformation is dependent on prior grain boundary deformation. Alternatives 2) and 3) would view grain boundary sliding as occurring in series with another deformation process which could be rate controlling. McLean prefers item 3) as the sliding basis,4 where subgrain rotation results from dislocation accumulation in the substructure at the grain boundary. Crussard and Friedel's5 treatment of grain boundary migration considers that dislocations are forced into the grain boundary and are dissociated into dislocations with Burgers' vectors nearly parallel to the grain boundary. The movement of these partial grain boundary dislocations then produces the sliding. The results of this investigation have indicated alternative 3) to be the most appropriate and it is this aspect of grain boundary sliding which will be analyzed. EXPERIMENTAL PROCEDURE Three types of tensile creep tests were employed in this study: (I) A constant load test of one very coarsegrained polycrystalline specimen at 500° F, 3600 psi, 1 pct per/hr strain rate to examine the grain and grain boundary orientation factors in grain boundary sliding. (II) Constant strain rate tests of polycrystalline specimens at 510o and 715o F, 2 pct per/hr strain rate to determine the grain boundary contribution to elongation at very low total strains. (m) Constant strain rate tests of bicrystals of various grain and grain boundary orientations at 500°F, 2 pct per/hr strain rate to obtain further information on the orientation effects in grain boundary sliding. The material used in the tests was a high-purity Al-1'.92 mg alloy, kindly furnished by Alcoa. Its composition is given in Table I. The alloy is a solid solution at the test temperatures. The coarse grained polycrystalline specimen for test (I) was prepared by recrystallizingthe machined specimen, straining it about 1pct intension at room temperature and annealing at 900°F for 8hr. The constant strain rate specimens (11), with an 178 in. sq. by 1/2 in. long gage section, were cut from 1/8 in. thick sheet of cold rolled and annealed (8 hr at 1000oF) material. The latter specimens were supported in a special jig during the milling operations to avoid any bending, and the gage section was subsequently heavily electropolished to remove the cold-worked surface layer. The bicrystals (ID) were machined in the same

Jan 1, 1963

By F. D. Rosi

The plastic properties of extended silver and copper crystals of varying purity were studied as a function of crystal orientation in the early stages of flow. Variations in the gross shape of the shear stress-shear diagram and in the properties of critical Variationsshear stress and shear-hardening coefficient were correlated with changes in slip-band developments. The phenomenon of work hardening is discussed in terms of the existing dislocation theory. IT appears certain from the early studies on the deformation characteristics in metal crystals1-3 that plastic flow takes place in a preferred crystallo-graphic slip system which is determined by the geometry of the crystal (law of maximum shear stress), and that the value of shear stress for this system is independent of crystal orientation (law of critical shear stress). Experimentally, it has been demonstrated further that the law of critical shear stress can be extended to include extensive plastic flow.&apos; Thus, the shear-hardening coefficient, which is defined as the slope of the shear stress-shear curve, also is considered to be independent of orientation. It is noteworthy that deviations from this empirical shear-hardening law have been reported in cubic crystals whose initial orientation favors slip on more than two systems.&apos; Moreover, this law appears to have been derived from stress-strain data relating to relatively high values of shear strain (0.5 to 4), where widespread slip and complex distortions can be expected, regardless of crystal orientation. Since existing data indicate that the strain inhomogeneity in a crystal is manifested particularly in the early stages of flow, it would appear that a more exacting test as to the fundamental nature of the shear-hardening law would be to investigate systematically the shape of the stress-strain curve as a function of crystal orientation in the earlier stages of deformation. With regard to the general form of the shear stress-shear curve for cubic crystals, early studies show a parabolic hardening law, where the shear 1 stress is proportional to the square root of the shear-strain. Since this law was predicted theoretically by Taylor" in his original dislocation model for hard- ening, it has been accepted widely as a fundamental flow characteristic of cubic metals. However, it was recently pointed out by Masing6 hat the parabolic law is not the elementary form of hardening in cubic crystals, but instead is a consequence of complexities in the flow process (e. g., deformation bands and unpredicted secondary slip). Thus, in the very early stages of deformation (< 2 pct extension) where the occurrence of such complexities is unlikely, a different strain-hardening behavior might be anticipated. This view is supported by the recent work of Rosi and Mathewson7 on high purity aluminum where a linear law was obtained for extensions up to 2 pct. A linear hardening over a wider range of deformation also was reported by Rohm and Kochendorfer8 ho deformed aluminum crystals under conditions approximating pure shear. Even more pertinent is the recent evidence of Masing and Raffelsieper9 on high purity aluminum crystals. It was found that for crystals having initial orientations near a <l00> or <1ll> axis, a high hardening was obtained, whereas crystals with a <110> orientation exhibited a low and linear hardening curve followed by a region of more rapid hardening. Since much still remains obscure concerning the details of strain hardening as well as slip-band formation in face-centered-cubic crystals in the early stages of deformation, the present study was undertaken to evaluate the effect of crystal orientation on these two important manifestations of glide. It is important to note here that at the time of this study, Lucke and Lange11 presented information on the orientation-dependence of the shape of the strain-hardening curve in aluminum of various purities. Their work, which essentially represents an extension of that of Masing and Raffelsieper, in many respects is parallel to that of the present study. Experimental Procedure Production of Single Crystals: Single crystals of silver and copper of varying purity were used in

Jan 1, 1955

By O. D. Gonzalez, H. A. Wriedt

Alloys ranging from pure iron to pure nickel were saturated with nitrogen gas at 918°, 999°, and 1217°C and analyzed. The solubility of nitrogen at 1-atm pressure was obtained as a function of nickel content for the whole range of iron-nickel alloys and the temperature dependence of solubility is shown for the experimental alloy compositions. The heat of solution and the entropy of solution of nitrogen in the alloys as func-tiom of composition up to 41 pct Ni are given. 1 HE acquisition of more exact thermodynamic information for systems composed of iron with various alloying elements continues to interest ferrous metallurgists. The interstitial alloying elements, especially carbon, hydrogen, and nitrogen, comprise a field of particularly intense study. A recent investigation of carbon solubility in Fe-Ni alloys held at 1000°C in gases of fixed carbon activity showed an unpredicted minimum in the solubility near 72 pct Ni.1 The present investigation was undertaken to see if a similar anomaly in solubility existed for nitrogen in Fe-Ni alloys. The solubility of nitrogen in ? iron at known nitrogen activities has been measured several times.&apos;-&apos; Corresponding information for the solubility of nitrogen in solid Ni and Fe-Ni alloys is not available. Juza and sachsze9 reported that metallic nickel dissolved 0.07 pct N in equilibrium with Ni3N at 445°C. This result was regarded as dubious by Turkdogan and Ignatowicz10 who found less than 0.0004 pct N in nickel specimens equilibrated at 600°C with ammonia-hydrogen mixtures having fugacities of N2 gas up to 35,000 atm. Such fragmentary reports indicate only that nitrogen gas has a very much lower solubility in nickel than in iron. MATERIALS A purified iron from Battelle Memorial Institute was used for solubility measurements. This grade contained more than 99.95 pct Fe, the highest content of any measured individual impurity being 50 ppm for each of As, C, Cu, and Pb. The nickel and iron-nickel alloys, supplied by the International Nickel Co., contained 0.02 to 0.04 pct C, 0.17 to 0.19 pct Mn, 0.04 to 0.08 pct Si, < 0.01 pct P, <0.03 pct S, and <0.20 pct Co as principal impurities. The Fe-0.59 pct Mn alloy was of zone-melted quality, the highest concentration of any individual impurity being 15 ppm Al. The "prepurified" grade of nitrogen gas from Matheson Co. had a nominal nitrogen content of 99.996 pct. An "electrolytic" grade of hydrogen gas from National Cylinder Gas. CO. in which the principal impurity is water vapor was admixed with the nitrogen to prevent oxidation of these specimens. This grade was preferred to a purer grade because the presence of some oxygen helps in suppressing contamination of the specimens, for instance, by silicon from the porcelain furnace tube. EXPERIMENTAL PROCEDURE The specimens were equilibrated in vertical tube furnaces through which a 99 pct N2-1 pct H2 gas was passed at ambient pressure. For the 915", 918", and 999°C runs, a wound-resistance furnace was used, and for the 1217°C runs, a furnace with a tubular silicon carbide element was used. The temperature control system on both furnaces was similar: a Weston "Celectray" controller with a modulator, responding to the electromotive force of a thermocouple with its hot junction in the furnace, switched the furnace current between high and low settings. The temperature distributions in the working zones of the furnaces were determined with calibrated Pt/Pt-10 pct Rh thermocouples. The overall uncertainty in temperature was estimated to be ±3° at 915° to 999°C and ±5° at 1217°C . Consideration of the small temperature coefficients of the equilibria studied, together with the error limits in the method of analyzing for nitrogen, showed that further refinement in temperature uniformity would give no improvement in resultant accuracy. The reactive gas was generated by mixing together "prepurified" nitrogen and "electrolytic" hydrogen directly from cylinders commercially supplied. The flow rates of nitrogen and of hydrogen were fixed by setting with bleeders the pressure drops across the individual calibrated flow meters of constant resistance. For any given alloy, the solubility of nitrogen at 1-atm pressure (% N) was obtained from the analyzed nitrogen content of equilibrated specimens (% Na)according to Sieverts&apos; law, thus

Jan 1, 1962

By J. K. Elliott, P. H. Kelly

Many engineering functions such as surface metering work and laboratory compressibility check points involve the use of liquid densities of light hydrocarbon mixtures at various pressures and temperatures. However, at the present time, no simple reliable method exists for determining density variation, particularly if the composition of the liquid is unknown. Consequently, a study was undertaken to develop and present a simple and accurate method of predicting density variation of a light hydrocarbon liquid with pressure and temperature, knowing only the density of the liquid at some condition. The experimental liquid compressibility data from API Project 37 by Sage and Lacey&apos; have been considered to be accurate within 0.5 per cent and cover a wide range of pressure (14.7 to 10,000 psia), temperature (100" to 400°F) and molecular weight (up to 150). From these data, a set of liquid density curves, which relate density to pressure, temperature and molecular weight, was developed. These curves make it possible to predict density variation with pressure and temperature. Compared to extensive laboratory compressibility data on a complex, light hydrocarbon liquid, the use of the liquid density curves resulted in an average error of less than 0.5 per cent. Based on the results of this analysis, it is concluded that the set of liquid density curves developed from the data of Sage and Lacey provides an accurate and simple method for predicting the density variation of light hydrocarbon liquids when the density at some condition is known. These curves should be very helpful in many engineering calculations, particularly in the surface metering of light hydrocarbon liquids. INTRODUCTION Many situations arise in field and engineering laboratory work, such as reservoir engineering studies, check of experimentally determined laboratory data and orifice flow-meter formulas, where liquid density factors at various pressure-temperature conditions are required. Also, the need for accurate light hydrocarbon liquid information has become more important with the advent of miscible-type displacements for secondary recovery purposes in oilfield operations. Several reliable methods are available1 - "or determining the density of liquid hydrocarbons if the composition of the liquid is known. However, there is a definite lack of methods for accurately determining the variation of density when the composition of the liquid is unknown. The purpose of this study is to review the various methods for determining hydrocarbon liquid densities and to develop a simple and reliable method of determining variation in density of light hydrocarbon liquids with pressure and temperature when the compositio~n of the liquid is unknown. METHODS FOR DETERMINING DENSITY OF LIQUIDS OF KNOWN COMPOSITION Sage, Lacey and Hicks&apos; have proposed a method to predict the density of light liquid hydrocarbons by using partial molal volumes. Data are available on experimentally developed partial liquid volumes of hydrocarbons over a rather limited range of temperature, pressure and composition. The partial mold volume method has proved satisfactory for determining the density of some hydrocarbon liquids when the composition is known. Within the range covered in the Sage, Lacey and Hicks1 data, the results agree within about 3 per cent of the experimental values. Hanson mentions the limitation of this method to a composition range of approximately 10 per cent by weight of methane, which will not allow this correction to cover most low molecular weight-light hydrocarbon liquids. Standing and Katz2 studied data on light hydrocarbon-liquid systems containing methane and ethane at high temperature and pressure and have presented a method for determining liquid densities, assuming additive volumes for all components less volatile than ethane and using apparent densities for methane and ethane. The compressibility and thermal-expansion curves used by Standing are based on assumptions that compressibility of a hydrocarbon liquid at temperatures below 300°F is a function of the liquid density at 60°F and that thermal expansion of the liquid is affected little by pressure. The information required to use this technique with an example problem is furnished by Standing.&apos; Hanson eports an average error of - 0.5 per cent using the method of apparent densities in calculating liquid densities of several volatile hydrocarbon mixtures. However, as implied, the apparent density method is not applicable for liquid density calculations when the composition of the liquid is unknown. Watson- as presented a method

By C. E. Hottman, R. K. Johnson

Fluid pressure within the pore space of shales can be determined by using data obtained from both acoustic and resistivity logs. The method involves establishing relationships between the common logarithm of shale transit time or shale resistivity and depth for hydrostatic-pres-sure formations. On a plot of transit time vs depth, a linear relationship is generally observed, whereas on a plot of resistivity vs depth, a nonlinear trend exists. Divergence of observed transit time or resistivity values from those obtained from established normal compaction trends rinder hydrostatic pressure conditions is a measure of the pore fluid pressure in the shale and, thus, in adjacent isolated permeable formations. This relationship has been empirically established with actual pressure measurements in adjacent permeable formations. The use of these data and this method permits the interpretation of fluid pres.rure from acoustic and resistivity measurements with an accuracy of approximately 0.04 psilft, or about 400 psi at 10,000 ft. The standard deviation for the resistivity method is 0.022 psi/ft, and for the acoustic method 0.020 psi/ft. Knowledge of the first occurrence of overpressures, and of the precise pressure-depth relationship in a geologic province, enab1es improvements in drilling techniques, casing progroms, completion methods and reservoir evalzmtions. INTRODUCTION CENKRAL STATEMENT Operators engaged in the search for and production of hydrocarbon reserves in Tertiary basins are more and more frequently confronted with complications associated with over pressured (abnormally high fluid pressure) formations. This is particularly true in the Texas-Louisiana Gulf Coast area. The problems associated with these formations are of direct concern to the combined activities of all phases of operations, i.e., geophysical, drilling, geological and petroleum engineering.&apos; - Knowledge of the pressure distribution of a given area of operations would greatly reduce the magnitude of many of these complexities and in some cases would completely eliminate specific problems. his pape; presents techniques developed for estimating formation pressures from interpretations of acoustic and electric log data. Specifically: the acoustical and electrical properties of shales, reflected by conventional acoustic and electrical surveys, can be used to infer certain reservoir properties, such as formation pressure, at any level in a well. It has been possible to develop these techniques because of a firm understanding of the basic principles that govern and apply to such overpressured provinces. NORMAL PRESSUKES Normal pressures refer to formation pressures which are approximately equal to the hydrostatic head of a column of water of equal depth. If the formations were opened to the atmosphere, a column of water from the ground surface to the subsurface formation depth would balance the formation pressure. On the Gulf Coast, the shallow, predominantly sand formations contain fluids which are under hydrostatic pressure. These formations are said to be normally pressured or to have a normal pressure gradient.* Experience has shown that the normal pressure gradient on the Gulf Coast is approximately 0.465 psi/ft of depth. OVERPRESSURES Formations with pressures higher than hydrostatic are encountered at varying depths in many areas. These formations are referred to as being abnormally pressured, abnormally high pressured, or overpressured. Formation pressures up to twice the hydrostatic pressure have been observed. These formations require extreme care and much expense to drill and to exploit. COMPACTION-FLUID PRESSURE RELATIONS THEORY The generation of overpressured formations in Tertiary sections of the Gulf Coast and several other Tertiary sedimentary basins is, in general terms, considered to be primarily the result of compaction phenomena.&apos; This portion of the paper presents a brief review of the theory which associates compaction and fluid pressure relations, and should thus provide the necessary background for an understanding of the techniques presented. See Hubbert and Rubey&apos; for a more comprehensive treatment of this subject. The theory of the consolidation of a water-saturated clay&apos; has been well established by workers in soil mechanics. The concept is explained by a model with perforated metal plates separated by metal springs and water and enclosed in a cylindrical tube. Fig. 1 is a schematic representation of such a model (see Ref. 5, Fig. 27, page 74). The springs simulate communication between clay particles, and the plates simulate the clay particles. Mano-

Jan 1, 1966

By O. R. Wagner, R. O. Leach

Immiscible displacement tests were performed in a consolidated sandstone core over the interfacial tension range from less thdn 0.01 to 5 dynes/cm to better define how interfacial tension (IFTJ reduction can lead to increased oil recovery. Data obtained were displacement efficiency at breakthbrough vs IFT for both drainage and imbibition conditions. These tests simulate water flooding under oil-wet and water-wet conditions, respectively. Results of the study have shown that displacement efficiency under both oil-wet and water-wet conditions can be markedly improved by a sufficient reduction in IFT. In the particular porous media used and for the low pressure gradients employed, the IFT must be reduced to a value less than about 0.07 dynes/cm to achieve increased recovery at the time of breakthrough of the injected phase. Below 0.07 dynes /cm, further small reductions in IFT result in large increases in displacement efficiency. Observed increases in recovery were obtained at pressure gradients which are well below those which can exist in the interwell area of a reservoir under water flood. The effect of pressure gradient on recovery is discussed. INTRODUCTION A residual oil saturation remains in rock which has been water flooded because, under usual reservoir conditions, the driving force which can be generated is inadequate to expel oil trapped by capillary forces. Since these capillary forces can be reduced by reducing the IFT a frequently studied method of increasing oil recovery has been the use of surfactants to reduce the water-oil interfacial tension. Mungan l observed improved recovery in both water-wet and oil-wet systems at 1.1 dyne /cm IFT, finding that the amount of improvement was greater in oil-wet systems. Moore and Blum,2 working with visual flow cell micro-models, con- cluded that recovery cannot be improved in water-wet systems by injecting surfactant solutions. They calculated that, for a pressure gadient of 1 psi/ft in their model, the IFT must be reduced to 0.03 dynes/cm to release oil trapped under water-wet conditions. Berkeley et al.3 indicated that, at representative field flooding rates, the IFT must be reduced to 0.001 dyne/cm to improve recovery, Thus, there is a wide variation of opinion about the IFT levels needed to improve recovery under field conditions. These previous investigators all have used as their experimental method the addition of surfactants to the injected water. The use of surfactant solutions to reduce IFT creates two experimental problems: (1) the loss of surfactant through adsorption on reservoir rock can obscure the true IFT value which exists at the displacement front, and (2) at very low values of IFT emulsifica-tion of oil and water commonly occurs. It is difficult, therefore, to determine whether the increased recovery is caused by IFT reduction as such, or is instead caused by emulsification. Also the properties of the available surfactants limit the IFT range which can be studied. In the present study the purpose is to better define how interfacial tension reduction can lead to increased oil recovery. A matter of great interest is the amount of recovery improvement potentially achievable in this way. The study was made using very low pressure gradients which was well within the range achievable by water flooding in the interwell region of petroleum reservoirs. A unique experimental approach was chosen to avoid adsorption and emulsification problems, and to allow convenient control of IFT. The fluid phases used were the equilibrium vapor and liquid phases of the methane-n-pentane system. The interfacial tension level was varied by changing the equilibrium pressure of the methane-pentane system over the range from 1,200 psia to near the critical pressure (2,420 psia). All tests were performed at a controlled temperature of 100F. The IFT-vs-pressure relationship for the methane-pentane system was based on the data of Stegemeier and Hough,6 and on new data obtained in this study. With this experimental approach it has been possible to study displacement at lower values of IFT than have been previously investigated.

Jan 1, 1967

By T. K. McCranie, A. H. Tousley, A. H. Kackman, L. R. Gregory, A. Jr. McElrath, R. J. Krekel

In Roman and earlier civilizations the term cement was applied only to mixtures of lime, pozzolana, sand, water, etc., used as a mortar to bind larger stones. Today, portland cement, the subject of this section, can be briefly defined as follows: The product obtained by finely grinding clinker produced by calcining to incipient fusion (i.e., sintering) an intimate and properly proportioned mixture of argillaceous and calcareous materials. History The Egyptians were probably the first to join building stones with a mixture of sand and a cementitious material (i.e., having the property of or acting like cement). It is generally accepted that the cement used by the Egyptians on such structures as the Great Pyramid was calcined gypsum, Later the Greeks began to calcine limestone for use as a mortar with sand and water. Still later, broken brick and tile were added to the mortar to make the first concrete. The Greeks and Romans found that some sands produced mortars that were especially resistant to the action of water. Hydraulic (i.e., underwater-hardening) cements formed by combining slaked lime, water, and finely divided siliceous materials (e.g., pozzolana) possess superior strength and are capable of resisting the destructive action of water. They were used on the Pantheon, Colosseum, and other structures, some of which are still standing. In 1756 an English engineer, John Smeaton, found that an argillaceous limestone (i.e., containing an appreciable amount of clay as an impurity) produced a cement with greater resistance to the action of water. Despite Smeaton&apos;s findings, the use of the old mixture of lime and pozzolana long retained its popularity. Significant contributions in cement technology from England, Swe¬den, France, and Holland were made in the next 68 years. However, the invention of portland cement is generally credited to Joseph Aspdin, an Englishman, who in 1824 patented "portland cement." The name was selected because, on hardening, it resembled the natural building stone from the Isle of Portland, England. The patent features mixing ground limestone and argillaceous materials in appropriate proportions and calcining (i.e., expelling CO2 by roasting) the mixture. This superseded the existing practice of calcining naturally occurring argillaceous limestone. In about 1845 Isaac Johnson, also English, conducted experiments on proportioning the components and calcining them at higher tem¬peratures. His accomplishments are accepted as the beginning of the present-day portland cement industry. The U.S. cement industry originated with the demand for good hydraulic cement for building structures such as the Erie Canal, which was started in 1817. The first discovery of cement rock (i.e., naturally occurring argillaceous limestone with near-optimum ratios of calcium carbonate, alumina, and silica) near Fayetteville, N.Y., was made by C. White. In 1818, White secured a patent for the manufacture of natural cement from that deposit. Subsequently, several natural cement plants were built in 1830-1840 at Rosendale, N.Y., and in the Lehigh Valley of Pennsylvania. David Saylor, who participated in establishing a natural cement plant at Coplay, Pa., in 1850 discovered that a superior cement could be produced by calcining the rock at higher temperatures than hith¬erto. In 1871, Saylor obtained a patent and commenced the manufac¬ture of portland cement. By 1890, there were 17 portland cement plants in the United States with a combined annual output of 62,300 tons. At the end of 1970, the number of plants producing portland cement in the United States (including Puerto Rico) was 169, down from a maximum of 185 in 1967, with total annual shipments of 73.4 million tons valued at $1,298 million. (Fig. 1). In 1970, annual world production of hydraulic cement (which includes pozzolanic materials, hydraulic limes, natural cement, alumina cement, and portland cement, all of which are in current use in various parts of the world) reached 630 million tons (Table 1). Flowsheets of typical U.S. cement plants are shown in Chapter 13. Chemical Composition and Physical Properties It is generally accepted that portland cement clinker consists of a mixture of compounds or synthetic minerals. The four principal compounds are:

Jan 1, 1985

By K. F. Veith, R. L. Marovelli, T. S. Chen

An analytical study is made of thermal stress distribution in a thin circular disc subjected to a peripheral thermal shock at various rates of heat transfer. The problem is of importance in predicting the thermal shock response of a rock body of finite size. The theoretical analysis is based on radial heat flow by conduction in the disc and heat exchange by convection between the disc and the surroundings. The case of constant properties and plane stress is treated. Solutions of the stress distribution are presented for both cooling and heating shocks and an average stress theory is formulated. Preliminary experimental verification was obtained from the results of shock tests on thin rock discs insulated on both flat end faces so that heat exchange took place through the exposed peripheral surface. Physical properties vital to the analysis are Young&apos;s modulus, tensile strength, coefficient of linear thermal expansion, thermal diffusivity and thermal conductivity. Plots of these properties are presented. Historically, thermal energy has been used for primary rock removal throughout the ages. Although it is not widely known, the fire-setting method of thermal rock fragmentation was still in use 100 years ago in systematic underground mining operations in Scandinavia.&apos; There, the availability of cheap labor and abundant wood fuel made the method competitive with the early blasting powders. By 1880, as high explosives replaced powder, use of the method declined and it was finally abandoned about 1885. Only 40 years ago, some experimental fire-setting methods were used for rock removal underground at Pribram and Zinnwald in Central Europe.2 Compressed air-oil burners replaced the earlier wood fuels. About 15 years ago, gaseous oxygen-oil burners were introduced in the United States and gained acceptance for difficult blasthole drilling and some quarry opera- tions. At present, there is renewed interest in the compressed air-oil burner designs. The literature included information on thermal secondary processes for rock weakening or particle liberation3,4,5,6,7,8 on thermal spallation of rock 9,10,11,12,13 and on the thermal fracture of materials other than rock. The 1955 Symposium on Thermal Fracture14 and the later work of Hassel-man, cover recent developments in thermal shock investigations on brittle ceramics. Although the number of published analytical and experimental investigations conducted on ceramic and refractory materials is large, the literature reveals that there is a lack of information on both the theoretical and actual response of rock to thermal shock. Many of the thermal shock studies on ceramic and refractory bodies are based on the case of heat transfer at the solid&apos;s surface by convection in either liquid or air. A similar heat transfer situation was adopted for a theoretical analysis of the thermal stresses in a thin circular disc subjected to a peripheral thermal shock. Experimental thermal shock tests were then conducted on rock specimens to check the analytical results. Specially insulated quartzite, basalt and taconite discs were shocked in either liquid or still air bath at various rates of heat transfer. The work was done in order to resolve the question as to whether theoretically determined tensile stresses are actually realized in a finite rock body undergoing thermal shock. Specifically, if theory predicts that the tensile strength of a rock should be exceeded in a particular type of controlled thermal shock, will fracture occur? This information is needed by Bureau researchers working on thermal and electrical rock fragmentation methods. The object of this paper is to present the main features of the theory and procedure being used in the authors&apos; approach to quantitative prediction of rock response to a thermal shock. THEORETICAL ANALYSIS In the analysis to follow, simple geometry of a thin circular disc is considered. The disc is assumed to be isotropic, homogeneous and perfectly elastic, and to have constant thermal and mechanical properties. The effect of radiation is neglected so that heat is transferred by conduction inside the disc and by convection with its surrounding. In addition, the end

Jan 1, 1967

By I. V. Baklashov

Geomechanical conditions of mining operation are determined by varying in time and space mechanical properties and initial state of the rock mass, by geological and technological factors. We define adaptive mining technology as a technology capable of adjusting to changing geomechanical conditions of mining operation. The ongoing research at Moscow State Mining University consisting of laboratory, theoretical, and field investigations aims at the development of theoretical basis and methodology of the system of geomechanical support of adaptive mining technology for the bedded salt deposit in the Urals, mined by room-and-pillar method. This system of geomechanical support is capable of - dynamically assessing mechanical properties and state of the rock mass varying within the panel; - mapping mechanical properties of the rock mass within the panel; - assessing and predicting mechanical condition of load-bearing elements of the rock mass and its changes due to the adjustment of the parameters of mining operation considering the in-situ geomechanical conditions.

Jan 1, 1996

By J. Lee, M. Peart, T. Bhambhani, D. R. Nagaraj, P. Riccio

"Over the past decade or so, our efforts have focused on developing the rationale and concepts for new technology in reagent development and optimization in the processing of base and precious metals. A major outcome of these efforts have been the development of a novel family of collectors, principally driven by the MAXGOLD® and Aero XD-5002® chemistries, for precious metals recovery from primary Au ores and Cu-Au ores. These chemistries was developed to be robust to address the complex mineralogy and gold deportment in these ores. Plant trial data for a variety of ores have confirmed that the both Aero® XD-5002 and MAXGOLD® chemistry are indeed versatile in recovering gold values occurring as gold alloys and/or associated with many types of sulfides, and in altering the deportment of certain sulfides (such as those bearing As, Bi etc). An overview will be given in this paper using plant data to highlight the application of these reagents.INTRODUCTIONThe subject matter of this paper is the flotation of Au containing minerals from their ores. The motivation from this manuscript comes from the several challenges faced with the processing of Au ores, as was articulated in detail by Nagaraj (2008). The biggest challenge is the complex mineralogy; most easy-to-treat free-milling ores bodies are largely depleted. The Au values are distributed in multiple host minerals such as pyrite, pyrrhotite, arsenopyrite and Cu minerals such as chalcopyrite. Au values also happen to be finely disseminated within the various minerals and are sometimes invisible in optical microscopy. Additionally, on any given day, some mines treat multiple ore types, and the mineralogy is different for each ore type.Xanthates continue to be the collectors of choice at most Au and PGM operations around the world. Most primary Au operations tend to consume very large amounts of collectors; the dosage ranges anywhere between 40-400 g/t and this has been attributed to both mineralogical and non-mineralogical factors (non-mineralogical factors include the low cost of xanthates and the mindset that “more is always better”, which is not necessarily the case). In addition, several studies now show that xanthates alone are never sufficient where multiple value minerals are present, and that supplementary collectors are required. The large doses present a substantial cost to the minerals industry, and many mining companies have expressed the need for more efficient reagents that can improve metallurgical performance at low dosages."

Jan 1, 2013

By Lifeng Li, Jhon Silva-Castro

In a previous work, the authors analyzed the overlapping probability of two adjacent charges in a single hole for pyrotechnic and electronic detonators. This document extends such work to a complete mine blast where more than two holes are detonated. In a mine blast, all the blast holes are connected as a network by detonators to follow a given initiation sequence. Such initiation sequence’s performance is based on the adequate timing between charges in the mine blast. The analysis of the reliability of a mine blast based on the timing between charges and the initiation type is presented in this document. For a long-run time and under proposed operating conditions, the reliability of the mine blast can be analyzed based on the network which is treated as a system. The failure of the system is defined as no success between any two delays charges either in a single hole or in between two holes.

Jan 1, 2016

By Donald W. Stever

In 1995 I was asked to participate in a litigation matter between a corporation and its insurance carriers concerning insurance coverage for remedial costs at a large, environmentally contaminated closed-down former industrial facility. One of the buildings on this site became known to the lawyers representing the company as “the infamous Building 8”. This building housed millions of documents retrieved from various locations at the facility while it was being shut down. It became apparent that the facility management had no document destruction policy, and thus Building 8 contained internal memoranda, notes, copies of correspondence, permits, operating records, inventory records, and the like from fifty years of operation. Needless to say, some of these documents, all of which were subject to discovery by the insurance companies in the litigation, contained material that was less than helpful to the company’s case. Of course, there were also a few helpful documents, but the overall usefulness of these records was outweighed by the negative impact they had on the conduct of the litigation. A second example involves e-mail. Several years ago, acting on an anonymous complaint that we later discovered was made by a disgruntled former employee who had been fired, a small army of federal environmental investigators descended on a client’s operating facility and, armed with a search warrant, literally commandeered the facility’s EH&S department. The investigators impounded the computers of the EH&S personnel and extracted all of the data from the hard drives of those PCs, as well as all EH&S related files from the hard drives of several servers used by the facility. These computers contained many years’ worth of stored e-mails, draft letters and memoranda, and other documents that provided grist for a four and one-half year criminal grand jury investigation of the facility and its EH&S staff. Both of these companies would have benefited from following a rigorous, enforceable, corporate records policy. Here is a third problem. My client had, during the 1960s, made a brief, and unprofitable foray into the nuclear fuel processing business. It ultimately sold the subsidiary, and was forced to give the purchasing company a broad indemnity against future liability. As might be expected, years later the facility was found to have considerable soil and ground water contamination both by chlorinated solvents and low-level radioactive material. Several years into the remediation program, my client discovered a tractor-trailer load of files, apparently removed from the subject facility, sitting in a parked trailer in a company-owned lot 300 miles away from the facility, where they had been for nearly thirty years. These documents were not helpful to the client, but had to be reviewed, at considerable cost, by paralegals. Moreover, several of the boxes turned out to have been mildly radioactive, setting off a chain of health and safety issues that consumed tens of thousands of dollars of legal expenses before they were resolved. Today, formal, enforceable corporate records management programs have become an extremely important element of overall corporate management. What was for most of the last century little more than a low level warehousing function is now a critical, actively managed, operating function that affects every level of corporate management. The rapid assimilation into corporate culture of electronic document management and the prevalence of e-email as the primary means of internal communication have created records management complexities the likes of which were not even conceived of fifteen years ago. Record preservation and destruction are no longer matters that can be handled on an ad-hoc decision making basis. Because of regulatory requirements affecting various classes of documents and the litigation consequences of ad hoc retention and destruction of corporate business records, and the need to have the ability to quickly retrieve documents in either a litigation or business negotiation context, a set of records management norms have evolved over time that have become the core elements of virtually every corporate records program. However, notwithstanding the existence of a set of norms (which are the basic elements of a

Jan 1, 2005

By Tom Tallone

In the majority of metal and nonmetal mining operations, narrow vein deposits are being mined with slusher hoists. Thin; method of mucking is costly, due in part to its inherent labor intense operation and to its inability to muck 100 pct of the deposits. Mechanized equipment would greatly improve the material handling in narrow vein mining and would dramatically reduce the operational cost. The Compact Loader/Trammer, known as the "mini-mucker" has been developed to increase productivity of the load/haul/dump portion of the typical narrow vein mining cycle. This is Volume II of the final report and concerns the operation and maintenance of the mini-mucker. Volume I covers a general and design review of the activities on the subject contract and are available under separate cover.

Jan 1, 1985

By Walter R. Curtner

Many, if not most, of today&apos;s pollution liability claims are related to events ("occurrences") that happened in the past. This fact creates an opportunity to obtain a large amount of insurance coverage at essentially no cost. Furthermore, in many cases, this insurance coverage is readily available. Scenario #1 For some 15 years, an underground gas tank has had a slow leak. The leak has now been discovered because the gas has contaminated nearby wells. As a result, an expensive $1 million cleanup is required. In addition, a liability suit has been filed for damages due to the contamination of nearby wells. Consequently, legal expenses are being incurred. Are all of these actual and potential costs insured? Obviously, if you have a pollution liability policy in place, the above costs will probably be insured. I say probably because business liability policies are not uniform. But, what if you don&apos;t have a pollution liability policy and what if your current general liability policy excludes all pollution liability (as most of them do today)? Under these circumstances, it first appears there is no insurance for this $1 million cleanup and liability suit. But this is probably not the case. You may well have insurance coverage, and you may well have much more insurance coverage than you ever expected. And, the insurance that I&apos;m referring to is already in place. You simply need to find it and learn how to use this insurance - I&apos;m referring to your old policies. In many cases, old liability insurance policies provide coverage for claims made today, because these policies were written on an "occurrence" basis of coverage. In fact, most still are written this way. This means that the insurance policy covers bodily injury or property damage liabilities (as defined in the policy) arising out of&apos; "occurrences" or accidents that happen during the policy period regardless of&apos; when the claim for damages is made. Therefore, for insurance purposes, the key question is: when did the "occurrence" take place? If someone falls and breaks a leg, that is clearly an "occurrence." The broken leg occurrence is, therefore, insured by the liability policy that was in existence at the time of the fall - regardless of when the claim or suit is filed, if ever. However, the answer to this question is seldom an easy one when you are looking at a pollution claim. In our scenario, the tank had a slow leak over 15 years, but property damage was not discovered until now. The question of when the "occurrence" (as defined in the insurance policy) took place has been litigated and continues to be litigated in many courts across the country. But, most often the answer has been that, for insurance purposes, the "occurrence" is the entire period that the tank was leaking (15 years), even though the contamination to the water was not discovered until 1987. This means that the person or company that is insured can potentially use all of its general liability policies (if they are "occurrence" policies, and most were), which were purchased during the 15 years from 1972 until 1987. And, these policies will potentially insure all of the claims and related exposures that arise out of this leaky underground gas tank. Scenario #2 In our first scenario, the claims and expenses were insured by past general liability policies because the claims arose out of events in the past, which, in turn, caused damage. Let&apos;s look at another example. In this scenario, Company XYZ has received a request to help clean up a landfill site because 10 years ago, XYZ dumped some toxic substances at the site, which was totally legal at the time. XYZ has not dumped anything at the site since this time. Nevertheless, XYZ is now being required to contribute $2 million to the cleanup of this site. In this scenario, if you had purchased "occurrence" general liability policies 10 years ago, these 1977 policies would (potentially) apply to the current $2 million cleanup claim. And, the reason is that the "occurrence" leading to the 1987 claim took place in 1977.

Jan 10, 1987

By F. A. Forward, A. H. Ross, J. Halpern

Application of the carbonate leaching process to carno-tite ores has often been limited by the difficulty of obtaining simultaneous high recoveries of uranium and vanadium. The chemical aspects of this problem are discussed and the effect of prior roasting procedures on this discovery is described. IN treating carnotite ores by carbonate leaching it is often necessary to subject the ore to a prior roast. Among the advantages that may result from roasting are: 1) improvement in settling and filtering characteristics of the ore; 2) destruction of carbonaceous impurities that would otherwise contaminate the leach solution and consume carbonate reagent; and 3) substantial increase in extraction of vanadium, which is usually low when the un-roasted ore is leached. Recovery of vanadium may be an important factor in processing carnotite ores, and the fact that vanadium is usually recovered in good yield by acid leaching has often been an economic advantage over results obtained with carbonate leaching. It has been found that response of an ore to carbonate leaching, following roasting, depends primarily on its composition and on the conditions of the prior roast treatment, particularly with regard to the roasting temperature, the atmosphere maintained above the charge during roasting and cooling, and the presence of certain reagents. These factors, especially the last, virtually determine the extractions of uranium and vanadium attainable by carbonate leaching, as well as the reagent consumption on leaching, whereas adjustment of the leaching conditions has only a limited influence. These variables were examined systematically to elucidate roasting and carbonate leaching of carnotite ores and to establish a treatment yielding high recoveries of both uranium and vanadium. Tests were conducted on samples of four different Colorado Plateau ores, described in Table I. Roasting Procedure: The roasting tests were conducted in an electrically heated furnace in which the temperature was controlled to ±15°C. The ore (usually a 500-g charge) was ground to —100 mesh, mixed with the desired reagent, and spread in a silica tray to a bed depth of about 1/2 in. During the roast the charge was rabbled at intervals of 15 min. To provide free access of air the furnace was usually ventilated; however, in a few experiments a controlled atmosphere such as carbon dioxide or hydrogen was maintained above the charge. Leaching Procedure: The pulp, generally comprising 500 g of ore and a 2000-cc solution containing 80 g per liter of Na2CO8 and 20 g per liter of NaHCO3, was agitated in an autoclave at 120°C, under 30 psi 02. Samples were withdrawn periodically, and the solution and ore residue were analyzed. Under the conditions employed, maximum attainable extractions were generally achieved in 4

Jan 1, 1959

By Peter Grandone

"INTRODUCTION The injection of water into partly depleted-oil-bearing formations as a means of supplying additional energy to flow oil wells now is recognized by the petroleum industry as an effective method of increasing the recovery of oil. The benefits to be derived from water-flooding oil sands were discovered accidentally more than 4o years ago, when oil producers in the Pennsylvania and western New York fields observed suustantial increases, in oil-production rates when water leaked past corroded casings of old wells into producing sands. This observation prompted some operators purposely to perforate or slit the casings opposite the producing formation in some of their wells to permit water to enter the formation. However, as many operators viewed the practice with skepticism and considered it to be in violation of oil-conservation principles,- systematic water-flooding was not initiated until the Pennsylvania legislature, in 1921, enacted a law authorizing water-flooding of oil sands in that State.Although water-flooding has been practiced in a haphazard manner for more than 25 years in Chautauqua and Montgomery Counties, Kansas, planned or systematic water-flooding in that State had its inception in 1935, when the legislature, following the example of Pennsylvania, also passed a lava/ authorizing water-flooding. The early operations and, to some extent, those still, practiced in the Chautauqua-Montgomery area consisted in raising or perforating the casing to allow water from upper strata to gravitate into underlying oil-producing formations. The extent to which this type of water-flooding affected petroleum production in the old stripper area of eastern Kansas is not known, but it is known to have increased oil production ap¬preciably from many leases.Following enactment of the law permitting water-flooding in Kansas, three operators inaugurated, in that same year, three organized flooding projects in three different counties of the southeastern part of the State. The first organized project on record was that of the York State Oil Co. in the Seeley pool, Greenwood County. On this project, the injection was started on May 15, 1935, into the Bartlesville sandstone at a top depth of 1940 feet."

Jul 1, 1944

By H. Foster Bain

(San Francisco Meeting, October, 1911.) [SECRETARY&apos;S NOTE.-This paper, presented in oral abstract, at the San Francisco meeting, was not at first supposed by Mr. Bain to be required for publication in the Transactions; and the excursion to Japan, in which he took part, immediately after the San Francisco meeting, delayed his presentation of the manuscript. After his return to San Francisco, Mr. Bain, in view of the importance of his paper and its discussion, kindly furnished it in full. The delay in its publication (since it was received in April last) has been due, partly to the circumstance that other contributions had meanwhile acquired the "right of way," and partly to the consideration that, the situation contemplated in Mr. Bain&apos;s paper having remained practically unchanged, the paper and its discussion would not lose force or timeliness by this lapse of time.-J. S.] No acute observer of public affairs can have failed to observe a growing disposition on the part of the public to change emphasis in government from political equality to social justice. When our own government was founded it was felt to be sufficient to secure to each individual the fullest possible freedom of opportunity, and such a scheme was excellently adapted to the rapid development of a large territory having a small population. As the number of people in a given area increases, there are more points of contact and conflict; each must move in a smaller orbit, and there must be more regulation. Germany is making faster progress in industry than is any other country. The principal reason is the insistence there on team-play. In Germany there are fewer multimillionaires and more socialists (spelled with either a big or little " S ") than in any other of the leading countries; but Germany wins trade and is steadily improving the conditions of life for her citizens. To some, the change from the freest individualism is welcome; to others it is intensely unacceptable. To this fundamental difference in view-point may be imputed much of the vigor with which the controversy regarding coal-lands has been waged. That present conditions in Alaskan coal-fields are extremely unsatisfactory is generally recognized, but there are wide dif-

Aug 1, 1912

By Niels Verbaan, Ernesto Bourricaudy, Ronald Molnar, James Brown, Sunil Jayasekera

"SGS Minerals commissioned an internal R&D program to develop in-house expertise to design, set up and operate REE separation pilot campaigns at its Lakefield, Canada site. A team approach was used that included expert consultants in the field of REE separation as well as in-house expertise supported by the on-site Analytical Laboratories.A mini pilot scale SX circuit was designed and constructed consisting of several modular banks of 30 stages each. About 80 stages of mixer-settlers were used to separate Pr and Nd from La and Ce contained in a synthetic REE chloride stream simulating the raffinate from an initial La-Nd|Sm-Lu+Y separation.Two pilot campaigns were operated totalling 25 days of 24/7 operation with 99.4% plant availability in the final 20 day campaign. Purities of > 99.9% in the Pr-Nd strip liquor and > 99% in the La- Ce raffinate were achieved and simultaneously sustained in the second campaign for prolonged operating periods. Key to controlling and adjusting the circuit was the rapid assay turnaround (as low as 2 hours) provided by the on-site SGS analytical lab. This permitted the operating team to modify conditions and observe the effect of changes relatively quickly considering the large number of stages. A portable XRF analyser was also used to track evolving assay trends in the circuit. The small physical size of the circuit enabled longer operation with a limited amount of sample.This paper discusses the design of the circuit, operating conditions, some of the key operating factors and controls and results obtained.INTRODUCTIONSGS Minerals commissioned the design of and built a solvent extraction (SX) pilot plant for the separation of rare earth elements (REE). The plant consists of a battery of 120 mixer-settlers set up in a dedicated piloting facility.The purpose of the programme was to develop capabilities and in-house expertise in REE SX separation technology. The program aimed to establish operating procedures, sampling regimes, and analytical methodologies and protocols for this type of process/plant. A team comprised of SGS personnel and several external consultants with prior industrial and REE separation piloting experience was assembled to achieve these objectives."

Jan 1, 2016