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By K. P. V. Lei

The Bureau of Mines investigated molten salt electrorefining 'n helium atmosphere cells as a means for the production of ductile vanadium. 'Electrolytes composed of NaCl-VCl2, LiCl-NaCl-VCl2, BaCl2-KCl-NaCl-VCl2 KCl-LiCl-VCl2, and CaCl2-NaCl-VCl2 were tested. Two electrolytes, KCl-LiCl-VCl2 and CaCl2-NaCl-VC12, were selected for laboratory-scale production tests. A molten salt electrorefining process was developed for the production of ductile 99.6 percent vanadium from a commercial 90-percent grade. Using the CaCl2-NaCl-VC12 electrolyte, an 87-percent recovery of ductile vanadium was made; an 85-percent recovery was made with the KCl-LiCl-VCl2 electrolyte.

Jan 1, 1967

By G. W. Nabor, A. S. Odeh

The effect of production history of a well on the results of two-rate flow tests, and conventional build-up analyses was investigated. The effect was examined by means of digital computers and an R-C network model, respectively, for wells with infinite and finite radii of drainage. For systems which behave as infinite, it was found that production history and the duration of production at constant rate prior to the initiation of the test have important effects on the results. During build-up time equal to about one-fourth of the stabilized time, correct permeability-thickness product calculations can be made. For wells with finite radii of drainage, the time was determined during which the straight line can be satisfactorily used for permeability-thickness product calculations in case of drawdowns and build-ups. On build-ups, the dimensionless time (based on the external radius) during which the straight line gives reliable results was detertriined to be about 1/12. This is one-fourth as long as that of the drawdown. The investigation was done theoretically, and subsequently was verified by R-C network model runs. General interpretive rules were formulated which, if not followed, could lead to serious errors. Moreover, a recommended testing procedure is reported. INTRODUCTION The method used by most reservoir engineers for estimating formation characteristics in a producing well is the analysis of pressure build-up data. The method originally devised by Horner' makes use of the point source solution to the diffusion equation. This solution is approximated by a logarithmic function and the superposition principle is employed to arrive at the well known pressure build-up equation:where q, the flow rate, is in reservoir B/D; ft is in cp; kh is in md-ft; At is the shut-in time; and t is the producing time. At and t are in any consistent time units. Ey. 1 is applicable to a well of unlimited drainage radius which produces at a constant rate q from zero to time t and is then shut in. Such a constant production rate seldom obtains in practice. Therefore. a correction term must be applied to Eq. I to account for the varying rate. Two theoretically accurate methods are available for treating the variable rate case. The first, originally derived by Horner,' is based on the application of the superposition theorem. It requires knowlege of production history of the well as a function of time and results in lengthy and laborious calculations. The second t*q* niethod is suited for short production tests and requires that the shut-in time be at least one and one-half times the production time. A third method which is not based on any theoretical justification and which was suggested by Horner as a "good working approximation" is the one used by the majority of reservoir analysts. especially when the well has been producing for a long time and the t*q* method is not practicable. The key to this method is in choosing or determining the t that appears in Eq. 1. Horner suggested using a corrected time t, in place of t. t, is calculated by dividing the total cumulative production by the last established rate. Therefore, a normal procedure of pressure build-up testing is to stabilize the well at a constant rate for at least 24 hours before shut in and to use the stabilized rate to calculate t,. The analysis is then made by plotting either or P. and examining the resulting plot for the expected straight line to calculate kh and the original reservoir pressure. Recently, Russell" proposed a method for determining formation characteristics from two-rate flow tests. His method reduces to pressure build-up if the second flow rate is zero. Russell uses the Horner simplified procedure for calculating a corrected t,. His method also requires the stabilization of the well at a constant rate q which is used to calculate t,. Theoretically, the above procedure is valid for a well with an unlimited radius of drainage or with a limited radius as long as the boundary effect has not been felt by the well. Several authors'' derived formulas which allow the estimation of time during which limited reservoirs behave as infinite ones and, thus, can be treated by unsteady-state mechanics. One equation derived by Swift and Kiel' terminates the application of unsteady-state theory when the drainage radius reaches one-half the reservoir radius. Thereafter, steady-state behavior obtains. Another equation derived by Jones'" initiates steady-state

Jan 1, 1967

By J. D. Marchant

The Bureau of Mines studied solid-state electromigration to determine the value of the technique as a method of purifying cerium metal. Cerium metal in bars 6 inches long and 1/2 inch in diameter was refined at 600° C by solid-state electrolysis to remove iron, copper, and manganese. Iron and manganese were electrotransported to the anode and copper was electrotransported to the cathode. The concentration of iron at the anode of a cerium bar was 800 times greater than the concentration at the cathode. The concentration of manganese at the anode was twice the value at the cathode. The concentration of copper was 170 times greater at the cathode than at the anode. A radiotracer technique was used to follow the iron migration in the cerium metal. Molybdenum, silicon, and aluminum impurities were not electrotransported.

Jan 1, 1967

By Frank E. Williams

This Bureau of Mines report deals with the urbanization of Tucson, Ariz., a southwestern city with an arid environment. Zoning regulations concerning known aggregate sources are described, and information relating to projected needs for the urban area is furnished. History of growth is outlined not only for the local aggregate industry, but also for the entire urban area. Past conditions are pointed out and background material for future conditions is provided.

Jan 1, 1967

By Jr. Blake

This work was done to determine the technical feasibility of using the Pedersen process to produce cell-grade alumina and an iron byproduct from the high-silica and titania bauxites of the Pacific Northwest. Smelting of these bauxites with lime and coke at about 1,750° C in an electric arc furnace produced calcium aluminate slags in which at least 80 percent of the alumina was leachable by sodium carbonate solution. After a lime-desilication of the sodium aluminate leach liquors, neutralization of these solutions with carbon dioxide resulted in precipitation of an alumina hydrate of sufficient purity for calcination to cell-grade alumina. Recoveries of byproduct iron averaged over 90 percent; however, the iron contained about 1 percent phosphorous and would require additional refining. Additional small scale tests on these slags showed the following: (1) Titania had little effect on leachability if sufficient additional lime was added to form calcium titanate (CaO.TiO 2); (2) a slag containing about 14 percent silica required a slower cooling rate than one containing 7 percent silica for formation of high percentages of soluble aluminates; and (3) high-silica slags leached better at room temperature for long periods than at 65° C for shorter periods, but low-silica slags leached well by either method.

Jan 1, 1967

By B. G. Agnew

In evaluating fracture treatments, the need to answer such questions as "What zone or zones were actually treated?" and "What was the vertical extent of the treatment" is necessary, since determining effectiveness of the fracture treatwrent depends on knowledge of the reservoir portions stimulated and the vertical extent of the fracture system or systems. Injection of hot or cold fluids during fracturing operations will transfer heat to the surrounding formations and fracture faces mainly by heat conduction. Once injection ceases, temperature anomalies will develop opposite the zone fractured because the rate of temperature decay is less than that opposite zones heated or cooled by flow inside the wellbore or along the cement sheath. Thus, temperature surveys can he used to determine where fractures were generated outside the wellbore and to reasonahly estimate the vertical extent of the fractrires. This technique has been used successfully to evaluate over 344 fracture treatments at depths ranging from 1,500 to 15,700 ft. Examples of actual temperature surveys are presented to show how this method of fracture treatment evaluation can be used effectively and beneficially. INTRODUCTION Stimulation of producing or injection wells by fracturing is commonplace in the industry today. In evaluating these treatments, two basic questions which arise are "What zone or zones were actually stimulated?" and "What was the vertical extent of the treatment?". Knowledge of the reservoir portions stimulated and vertical extent of the fracture system or systems is vital to effect efficient and economical well completions and to assure maximum recovery from reservoirs. Not all fracture treatments are successful and many times the desired or anticipated results are not achieved. When this occurs, it is in most cases the engineer's job to determine why. The answer to this problem forms the primary basis for deciding whether to spend more money for development drilling and/or completion attempts or to forego additional expenditures to improve the particular zone. Also, knowledge of the reservoir portion actually stimulated is invaluable in planning future workovers. This is especially true in wells producing from reservoirs containing multiple porosity stringers or zones. For various reasons, all zones within a reservoir may not be perforated on initial completion with the thought of developing remaining zones through future workover operations. Because particular zones are perforated and fracturing fluid pumped down the wellbore, it cannot be assumed that all perforated zones are stimulated, and in turn drained. Occasionally, unperforated zones which are planned for future development are actually stimulated on initial completion. eliminating the need for future recompletion attempts or all zones perforated initially are not stimulated, thus requiring additional completion work to insure that these zones are adequately drained. In most cases, it is costly. if not impossible, to determine with assurance why a fracture treatment is unsuccessful after the job has been completed and the results tested. Further, unpredictable upper and lower fracture barriers. as well as possible borehole communications (cement channels), do not permit it to be taken for granted that the formation opposite the perforations is the only zone receiving the fracture treatment. Thus. evaluation of fracture treatments is necessary for efficient and prudent well completion practices and should be done simultaneously with the fracture job. Several methods have been used to locate fractured zones, all of which are based on detection of radioactive tracer materials added to either the fracturing fluid or the propping agent. These methods have been helpful in increasing knowledge of fracturing operations; however, they are seriously limited because of cost and inability to detect accurately radioactive tracer material more than a few inches away from the borehole. To develop a better diagnostic tool to pinpoint which zone or zones had actually been fractured, temperature surveys were run after fracturing with heated and cooled fluids. Significant temperature anomalies were found to exist opposite zones suspected of receiving the fracture treatment. From the analysis and examples to be shown, it can be seen that temperature surveys run in a stabilized wellbore several hours after a fracture treatment using hot or cold fluid will yield temperature anomalies which show the actual reservoir portion stimulated, the vertical extent of the fracture system or systems and a qualitative indication of the portion of fracture-fluid volume entering a given depth interval. The experience and illustrations used in this paper are based on evaluation of over 344 fracture treatments during the past three years using this diagnostic tool at depths ranging from 1.500 to 15,700 ft and fracture volumes ranging from 2.000 to 110.000 gal. Based on analyses of these temperature surveys, analyses of fracture gradients and evaluation of several open-hole packer impressions in the West Texas area,' vertical fracturing is the predominant mechanism and horizontal fractures occurred frequently, if at all.

Jan 1, 1967

By F. M. d’Heurle

Films of molybdenum have been prepared by sputtering onto oxidized silicon substrates. The resistivity. lattice parameter, orientation, and grain size were studied as a function of substrate temperature and substrate bias. Under normal sputtering conditions, the resistivity of the films was found to be quite high (600 x 10 ohm-crn). However, with the use of the negative substrate bias of 100 v and a substrate temperature of 350°C, films weve produced with a resistivity of ahout twice that of bulk molybdenum. The lattice parameters measured in a direction nornzal to the surface of the films weve found to be gveatev than the bulk value. This was interpreted as being at least partly due to the presence of compressive stresses. The effects of annealing in an Ar-H atmosphere were studied in terms of diffraction line width, lattice parameter, and resistivity. BECAUSE of its relatively low bulk resistivity (5.6 x 106 ohm-cm)' molybdenum is potentially interesting as a thin-film conductor in integrated circuits. An additional feature which makes it attractive for this purpose is its low coefficient of expansion (5.6 x KT6 per "c),' which is fairly well matched to that of silicon (3.2 x 10 per c). It is possible to deposit molybdenum films by evaporation but generally films produced in this manner have a high resistivity. In order to achieve resistivities close to bulk value, Holmwood and Glang found it necessary to operate in a vacuum of about 107 Torr and to maintain the substrates at 600 C during film deposition. Sputtered molybdenum films have been examined by Belser et a1.7 and, recently, by Glang et al.' This paper describes the results of an attempt to extend some of that work and examine the effects of annealing and getter sputtering on the physical and structural properties of the films produced. SPUTTERING APPARATUS AND PROCEDURE The apparatus used for most of the film sputtering work described here consisted of two "fingers" serving as anode and cathode, respectively, which were mounted within an 18-in.-diam glass chamber. A liquid nitrogen-trapped 6-in. diffusion-pump system was used to achieve a vacuum of about 1 x 107 Torr within the chamber prior to sputtering. The essential features of the equipment are shown in Fig. 1. Cathode and anode fingers are stainless-steel tubes isolated from the top and bottom plates by Teflon collars. In order to limit the discharge to the space between anode and cathode, each finger is surrounded by an aluminum hield, at ground potential, having an internal diameter 18 in. larger than the outside diameter of the finger. The cathode and anode fingers are 6 and 4 in. in diam, respectively. A 116-in.-thick sheet of molybdenum is brazed with a 10 pct Pd, 58 pct Ag, 32 pct Cu alloy to a copper disc which is mounted by means of screws and a large 0 ring onto the lower end of the cathode finger. The disc is cooled during sputtering by water circulation inside the finger. The use of several feet of plastic tubing for the water input and outputg reduces leakage to ground to less than 1 ma when the cathode potential is raised to 5 kv. The upper end of the anode finger is terminated by a brazed-on copper block. A variety of specimen holders can be easily mounted on the upper face of this block. Substrate heating or cooling is achieved by use of an appropriate unit attached to the lower face of the same block. Heating is achieved by means of cartridge-type heaters and cooling by copper coils fed with forming gas under pressure. The inner chamber of the specimen finger constitutes a small vacuum chamber of its own which is evacuated by an auxiliary mechanical pump in order to limit heating element oxidation and heat transfer by convection currents. An advantage of the finger arrangement is the absence of cooling and heating coils and wires within the main chamber. The stain less-steel shutter is useful to establish a discharge for cleaning the cathode at the beginning of each sputtering run. Water cooling of the shutter reduces heating and the out-gassing of impurities which might condense on the nearby substrates. Unless otherwise specified, the substrates used in these experiments were 1-in.-diam oxidized silicon wafe:s, 0.007 in. thick, having an oxide thickness of 6000A. The substrate holders were large copper discs onto the surface of which a number of molybdenum discs, 116 in. thick and 78 in. in diam, were brazed. The wafers were clamped to the molybdenum discs

Jan 1, 1967

By J. E. Hilliard

AS is well-known, the length per unit volume, Lv, of any lineal feature (such as grain edges in a polycrys-talline specimen) can be estimated from a count of the number of point intersections with a random plane of polish. Specifically:' Lv = 2NA in which NA is the expected number of intersections per unit area of the plane. As with all other measurements in quantitative metallography, the estimation of Lv is subject to a sampling error, the magnitude of which will depend on the number of observations. The analysis is usually performed by counting the number of intersections falling within a closed test figure of known area applied to a succession of different areas on the plane of polish. The test figure can be drawn directly on the screen of a projection microscope or else superimposed on the image of the structure by means of a reticule in a focusing eyepiece of an ordinary microscope. The use of micrographs is very inefficient unless, as in the present study, these are also needed for some other purpose. Consider an analysis in which n applications are made of a test figure within which the expected number of intersections is N. The expected total number of intersections counted is then given by NT = nN If (N) is the standard deviation in N for one application of the figure and if the latter is applied to non-overlapping regions so that the N's are independent in the statistical sense, then the standard deviation in Nt is given by: a(NT) = a(N)vn Eliminating n from Eqs. [2] and [3] we obtain: Thus, k will be a constant for a given specimen and test figure. From Eqs. [ I] and [4] we find As is to be expected, therefore, the fractional error in the estimation of Lv is inversely proportional to the square root of the total number of intersections counted. It is very desirable to have at least a rough estimate of k before starting an analysis, since it will then be possible to decide in advance by use of Eq. [5J how many counts should be made in order to achieve the desired accuracy in Lv. Without such information the investigator, unless lucky, will either do needless (and tedious) work or else obtain a result with too large an error. It is very easy to calculate k for the limiting case of N — 0, i.e., when the test figure is vanishingly small. In this case there is a negligible probability of two or more intersections falling within the figure. There are therefore only two possible outcomes: a count of one with a probability of, say, p and a zero count with a probability of (I-p). Thus and Therefore: We might expect k to depend on N and therefore on the size of the test figure. Such a dependence was observed2 in the analogous case involving the estimation of grain-boundary area per unit volume by a count of the number of intersections of a test circle with traces of the boundaries on the plane of polish. In this case the theoretical value of k at the limit N — 0 was 1.41. It was also predicted that k would display an initial sharp decrease with increasing N. Experimentally, k was observed to decrease to a value of 0.62 at N - 6 and thereafter remain approximately constant. Furthermore, the value of k for N > 6 was found to be insensitive to the form of the structure provided no pronounced anisotropy or grain-size variation was present. In order to determinewhether k would exhibit a similar dependence on N in the estimation of grain-

Jan 1, 1967

By Jr. Koch

As a part of a larger study of the distribution of metals within ore deposits, the geometry of distribution of gold, silver, lead, copper, and zinc in five veins of the Fresnillo mine, Zacatecas, Mexico, was established. The purpose was to obtain basic data necessary for evaluation of geological theories about processes of vein formation and useful for practical mining applications in ore estimation and prediction of ore beyond present workings. The Bureau of Mines investigation comprised statistical analysis of 64,000 assay values from some 16,000 mine samples. The samples were taken at 2-meter intervals in drifts exposing the veins through a vertical range of some 750 meters. Within individual veins, the metals are distributed in dome¬like patterns with highest metal contents tending Lo occur in oreshoots at the centers of the developed parts of the veins. However, in the block of ground containing all five veins, base metals define mathematical domes with highest contents near the center; precious metals define mathematical basins or troughs with low contents near the center. The ratio of silver assay values to lead assay values corresponds to two geographically distinct types of mineralization: one in which silver is closely related to lead, and another in which silver is independent of lead. Other metal ratios also vary regularly from one place to another. The statistical methods employed in this study would be useful for other geologists or engineers who need to analyze large amounts of assay or similar numerical data.

Jan 1, 1967

Over half of the molten aluminium produced at the 52,000 tons/ year eapacity plant operated by Comalco Aluminium (Bell Bay) Limited in Tasmania is cast into saleable produets by the direct chill process. Considering the importance of direct chill casting to the aluminium industry it is surprising that so little published literature on the subject is available, although Easton (1947), Smart (1954), and Uppert (1940, 1944, 1945) have contributed much toward lifting the veil of secrecy surrounding the process.The direct chill, or D.C. process as it is commonly called when related to aluminium, consists basically of feeding molten aluminium or its alloys into; water-cooled mould from the bottom of which solid aluminium is continuously extracted. Although the casting procedure is continuous in principle, the equipment is normally operated in an intermittent manner. Castings up to 20 ft long are formed during a cycle. At the end of the cycle casting is stopped and the pit into which thc castings are dropped is cleared before a new cycle commences. Depending on the size of the casting in relation to the cross sectional area of the pit and the support mechanism (commonly a hydraulic ram), 'drops' of up to 15 tons are not uncommon. This method of D.C. casting IS termed vertical D.C. casting and is the one most commonly employed in the aluminium industry.Horizontal casting has come more to the fore in recent years with the casting being extracted from the mould in the horizontal plane and is a truly continuous casting method since flying saws can be simply used to cut the continuously cast shape into required lengths as it emerges from the mould...

Jan 1, 1967

By W. Gordon Muir

This paper deals with the exploration, development and current operations of the salt mine at Goderich, Ontario operated by the Sifto Salt Division of Domtar Chemical Limited. The rock salt is obtained from a bed 1,760 feet below the surface, 75 feet thick, extending under Lake Huron. Annual production is in excess of one million tons. Large mobile equipment is used. Details of this equipment, as well as the shaft layout, which permits the equipment to be lowered underground with a minimum of trouble are outlined. Mining, crushing and screening procedures' are rev1ewed. Reference is also made to productivity salt distribution and uses.

Jan 1, 1967

By Janos de Warga

"After a short introduction to the history of the semi-conductor theory, the paper describes the principles of electron and hole flow in the semiconducting materials, the operation of the PN junction, and the rectification process in multi-layer devices (diodes and SCR's). The various methods of purification and zone-refining of the silicon are illustrated prior to the discussion on the most commonly used junction-forming processes (alloying, diffusing, etc.). Modern device fabrication and packaging operations are illustrated. Factory testing, evaluation, electrical parameters and guaranteed rating characteristics are listed. It is explained in this paper how the various device parameters affect the electrical performance of the finished unit and how the finished unit characteristics (turn-on, turn-off time, etc.) will influence the equipment rating. In concluding, some typical items of equipment are highlighted, and the applications of these semiconductor rectifiers in the chemical, mining, pulp and paper, and steel industries, etc., are dealt with."

Jan 1, 1967

By W. H. Young

The thickness of the coal seam is one of the more important items influencing the productivity and general overall efficiency of operation of a coal mine. The average thickness of coal seams mined in the United States has changed very little in the past 40 years. The first measurement of thickness of bituminous coal and lignite seams was made for 1920, when the average thickness was 5.3 feet.2 The average thickness for later years was as follows: 1945, 5.4 feet; 1950, 5.3 feet; 1955, 5.2 feet; 1960, 5.3 feet; and 1965, 5.2 feet.3 Table 1 includes data on number and production of bituminous coal and lignite mines classified by 1-foot intervals of seam thickness mined in 1920, 1945, 1950, 1955, 1960, and 1965. Though bituminous coal and lignite are mined today from seams of exceedingly variable thickness--less than 2 feet to more than 50 feet--a large majority of the production, 62 percent in 1965, came from seams 3 to 6 feet thick. This is not surprising since the coal seam of moderate thickness presents the least mining difficulties.

Jan 1, 1967

By W. O. Philbrook, R. H. Spitzer, F. S. Manning

A generalized mathematical model has been developed to describe the kinetics of the gaseous, topo-chemical reduction of porous hematite spheres. Gas-solid reduction is permitted at each of three advancing interfaces and is controlled by a complex series-parallel sequence of chemical and transport steps. Despite the fact that transport resistances are significant to the advance of each interface, little deviation from linear advance is predicted for the first 98 pct of reduction. Calculations to predict the movement of magnetite /wustite interface by a solid-state diffusion mechanism have been incorporated into the earlier dense-pellet model.' The porous-pellet model is found to give a better description than the dense-pellet one for McKewan's measurements2 of interface movements in dense polycrystalline hematite reduced in hydrogen-water vapor mixtures. THIS paper reports a continuation of work"3" directed toward the better understanding of gas-solid reactions and the development of mathematical models that may be helpful in the design or control of ore-reduction processes. Laboratory studies of the reduction of single oxide samples in tube furnaces normally employ an abundant excess of pure reducing gas. Reduction may appear to be adequately described by a model assuming gas-solid reaction solely at the iron/wustite interface.''' However, when iron ore is reduced in either a fixed bed or an efficiently operated counter-current column, there are portions of the bed where the partially spent gas is no longer capable of reducing wustite to iron. Nevertheless, the formation of the intermediate reaction products, wustite or magnetite, can and does continue. In order to account for this aspect of the reduction of beds of particles, three semiempirical mathematical models were devised.' One of these was for the limiting case of completely dense particles, and two alternatives were provided for porous particles. For purposes of the analysis, a dense pellet was defined as one in which the wustite and magnetite layers were impervious to the reducing gas when the atmosphere was capable of forming iron. In a porous pellet, the intermediate product layers were assumed to be sufficiently permeable to allow reducing gas to penetrate beyond the iron/wustite interface to form wustite and magnetite by removal of oxygen as a gaseous product rather than by a solid-state redfiction mechanism. Further progress required a better understanding of the reaction of the individual particles with the gas stream. A comprehensive mathematical treatment was developed' to describe the continually changing interplay of transport and reaction steps

Jan 1, 1967

By G. Bonnivard

"A complete laboratory process for the treatment of lateritic ores containing a high proportion of iron, as well as chrome and alumina, has been established. The ores treated originate from the tropical zones and result from superficial climatic alteration. According to recent estimates, the known reserves of such ores reach many billions of tons, thus representing huge potential reserves for the elements they contain.The process used is based on the alkaline roasting of pelletized ore in the presence of sodium carbonate. This treatment results in the separate recovery of pellets of upgraded iron ore, pure chrome oxide and hydrated alumina. The research described in the paper aims at determining the best experimental conditions for obtaining the highest extraction of the required oxide from this type of ore."

Jan 1, 1967

By John Sasadi

The mining industry depends upon inexpensive water transportation. Today, large quantities of mined products are transported by ships over oceans, from continents to continents, over lakes and waterways to the ultimate users. Sometimes, the routes these Bulk Carriers travel cover only a few hundred miles, sometimes thousands of miles halfway around the world. Most of the products of the mining industries are relatively inexpensive. A significant portion of their cost to the ultimate users are in the cost of transportation and not in loading and unloading these commodities at the ports of origination or destination. So far, the industry has produced very efficient loading and un- loading installations, but has very little influence over marine transportation or the design of the vessels themselves. Very little was ever published dealing with integrated transportation systems properly correlating all phases of the operation; namely, loading, marine transportation and unloading bulk materials.

Jan 1, 1967

By J. J. Demeter

A tube-wall reactor with a Raney nickel catalyst deposited on the outer wall of the tube by flame spraying is effective in the practically complete conversion of 3H2+1CO synthesis gas to a high-Btu gas (methane) at an hourly space velocity of 7,000 volumes of gas (NTP) per hour per volume of annular volume. Partially reacted synthesis gas containing an appreciable amount of methane can also be treated in this reactor to increase the heating value to over 900 Btu per cubic foot. Excellent heat removal through the metal wall to a coolant and temperature control were obtained. The heat transfer co-efficient from the catalyst to the coolant was about 275 Btu per hour per square foot per ° F. Synthesis tests were conducted with tubes 1.2 inches in ad by 6 inches long, and 1.3 inches in od by 36 inches long. When operating at a synthesis gas rate of 100 to 120 scfh per square foot of catalyst-coated tube, catalyst life was long enough to realize a catalyst cost for the raw Raney nickel alloy of about 0.3 cent per 1,000 cubic feet of pipeline gas (900 to 950 Btu per scf). Gas recycling at ratios of 1:1 to 3:1 was effective in increasing conversion and in extending the life of the catalyst to about 16 weeks. In cost and in operating characteristics the tube-wall reactor compares favorably with the fluidized-bed and hot-gas-recycle reactor systems for the synthesis of high-Btu gas from H2+CO.

Jan 1, 1967

By Robert M. Asimow, Bisuddhi Riddhagni

THE use of back-reflection Laue photographs for crystal orientation is standard in many research projects. The time required for the orientation of any given crystal depends largely on luck and the skill of the investigator. In any case, where large numbers of crystals are used, this time can be quite considerable when the standard methods involving a Greninger chart and Wulff net are employed. For this reason the technique described below was developed. This new procedure applicable for cubic crystals (without preparation of new charts) largely eliminates the skill and luck factors and makes possible the determination of orientation in minutes. The procedure works in the following way: the Laue photograph is examined and arbitrarily an important hyperbola is picked out. An important hyperbola is defined as one which contains some spots through which several hyperbolas pass. Such a hyperbola inevitably corresponds to a low-index zone axis. The angles between the reflection planes causing all the spots on this hyperbola can be read directly from a Greninger chart in the usual manner. If the hyperbola contains more than five spots, these interplanar angles will positively identify the zone axis and the indices of each of the reflecting planes. However, initially since neither the zone axis nor the Miller indices of a diffraction spot are known, there are a very large number of possibilities that must be considered. Using tables of interplanar angles to check out every possibility would be quite tedious, so that this approach is not generally used. Instead, various poles are plotted on a stereographic projection. In the cubic system, however, it is possible to plot out once and for all the angles between all planes of a particular zone axis up to some upper limit of Miller indices. This has been done for all low-index zone axes in Fig. 1. Given these charts, it is quite a simple matter to identify the spots of the unknown hyperbola. All that is necessary is to plot the angles read off the Greninger chart to the same scale as Fig. l(b) on a strip of paper. Then this strip can be slid along each zone axis of Fig. l(a) until a good fit is obtained. Once this is accomplished, the Miller indices of each spot are given and thus the orientation problem is solved. To check, it is possible to pick a second hyperbola and see whether a compatible solution is obtained. This is most conveniently done by picking for the second hyperbola one that contains a spot common with the first. If the specimen axis is chosen parallel to the incident X-ray beam, then usually the [ loo] hyperbola will appear on the film as one of the more important hyperbolas and consequently will be either chosen initially or as a check. Using the [100] hyperbola, after the (001) or (011) spots have been identified, the latitude and longitude of the specimen axis can be read directly from the Greninger chart so that it is unnecessary to use a Wulff net for the entire orientation procedure. This makes the operation not only quicker but more accurate. Of course, if neither the first nor second hyperbolas correspond to [loo] then a third hyperbola can be chosen.

Jan 1, 1967

By D. J. Crawford

The Lucerne Valley Operations of the Minerals, Pigments and Metals Division of Chas. Pfizer & Co., Inca, are located about 5 miles south of the town of Lucerne Valley, California. These operations consist of several limestone quarries, a whiting plant which produces finely pulverized limestone products, a-kiln which produces granular quicklime and lime products, and maintenance shops, warehousing, shipping, and office facilities. Construction of the Lucerne Valley plant began in 1961 as the result of a decision to utilize large undeveloped reserves of limestone in that area. Quarry development was started in the following year; and by 1965, Lucerne Valley had become the principle limestone and lime facility of the Western Operations of the Minerals, Pigments and Metals Division.

Jan 1, 1967

By E. L. Day

"In the early 1930s during the course of test work with a simple gold ore, it was evident that the time required to dissolve the gold by cyanidation was very much longer than should have been needed theoretically for the maximum size gold particles in the ore, A similar conclusion appeared to be valid for other gold ores. In a cyanidation system there are many factors which can influence the dissolution rate of gold, and a decision was made to investigate the more obvious variables, because a literature survey at the time showed that with the exception of the work of Yamazarki on the dissolution of silver in cyanide solution, virtually no attention had been given to this subject, Our work was not reported because the intention was to do this on completion of the Study, but owing to the demands on the Section's personnel for other work the investigation was never completed. Although other investigators have since studied the problem, the methods which we adopted and some of the conclusions may be of interest to metallurgists concerned with gold ore treatment.Form of GoldExperiments with gold ores were not possible because of the number of uncontrollable variables present in a gold ore-cyanidation system, therefore pure metal and reagents were used. Initially some experiments were carried out with gold leaf, but it was soon apparent that metal in this form was unsuitable because the uneven thickness of the leaf caused it to break up into pieces and. there was difficulty in determining precisely when complete dissolution had taken place, Numerous factors both expected and unexpected were found to influence considerably the results and much experimental work was necessary to establish the procedures which were finally adopted, Experiments were carried out with gold in the form of foil, wire, rings and sols. Finally, gold foil in the form of cylinders was adopted for most of the experiments although some work with gold in the sol form was included in the programme. Also some experin1ents were carried out with a gold ore to see if effects which were obtained with sodium chloride on gold sols were applicable to gold ores."

Jan 1, 1967