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By C. P. Lawhon, J. P. Simpson, W. M. Evans

Recent efforts to design drilling fluids for increased drifting rates have confirmed some laboratory results of other investigators, but have also produced additional data that should be considered. These data were obtained under controlled test conditions using a microbit drilling machine. Clays and some polymers have previously been reported to cause reduction in drilling rate. Recent data have shown that under laboratory conditions, suspensions of a single day or polymer have sometimes given faster drilling rates than when water was used. Measurements have been made of clay suspensions and polymer suspensions comparing filtration (I) under API conditions, (2) while drilling with temperature of 150F and differential pressure of 1,000 psi and (3) under dynamic conditions after drilling. Some correlation between instanraneous filtration (white drilling) and drilling rate has been observed. INTRODUCTION Several papers have been presented that related drilling fluids to penetration rate. Generally, it was found that a decrease in the solids concentration resulted in significant increases in the drilling rate. Of course, this change also resulted in a decrease in the viscosity of the drilling fluid.' Conclusions from investigations by this laboratory are in agreement. Data have shown that of the simple mud measurements commonly made at the drilling rig (density, plastic viscosity. yield point, API filtrate and total solids), only the density and total solids have a significant relationship to the drilling rate in Berea sandstone when attempting to correlate a single mud property individually.' More recent drilling rate experiments have been designed to study (1) effects of individual clays and polymers on drilling rates in Berea sandstone and Lueders limestone, (2) the relationship between drilling rate and dynamic filtration as measured after drilling and (3) the relationship between drilling rate and dynamic filtration as measured during drilling. Data show that drilling rates are dependent upon type and concentration of particles, type of formation and filtration of the individual fluids while drilling. Mud pressure: pressure of drilling fluid as measured after leaving the drilling chamber (Fig. 1). This is taken to be approximately the mud pressure just past the bit and at the face of the formation. Terrastatic pressure: pressure representing weight of overburden. Formation pressure: pressure of formation fluid as measured at outlet of drilling chamber (Fig. 1). This is taken to be approximately the pressure of fluid in the interstices of the formation. Differential pressure: difference between the mud pressure and formation pressure. LABORATORY EQUIPMENT AND TESTING PROCEDURE The drilling equipment was described in two previous publications."' Main components are a drilling chamber, filter-heater, rotary drive and variable-speed circulating pump. Auxiliary pumps supply pressure boosts for the mud, terrastatic and formation pressures. All equipment is designed for 15,000 psi and 500F. Capacity of the circulating system is approximately 7 gal. The mechanical design was facilitated by moving the rock down onto the bit. Data collected with this design should not differ from that obtained by a normal design where the bit moves into the rock. Drilling fluid is pumped through 50 ft of ID pipe coiled in an oil bath, enters the rotary shaft at a right angle and is pumped through the jets on the bit (Fig. 1). Most of the drilled solids are extracted by a screen mounted in the circulating system on the suction side of the pump. Data reported in this paper were obtained by controlling these parameters: mud pressure, 5,000 psi; formation pressure, 4,000 psi; terrastatic pressure, 5,000 psi; force on bit, 1,000 Ib; formation, Berea sandstone and Lueders limestone; flow rate, 7 gal/rnin; bit, 11/4-in. diameter with two 0.078-in jets; mud temperature. 150F; and rotary speed, 60 rpm. Mud pressure was controlled at 5,000 psi, thus giving a differential pressure of 1,000 psi even though the fluid densities varied. Cores of 3%;-in. diameter and 8 in. long were selected from quarry blocks to provide some control of grain size distribution, permeability and porosity. A 2-in. section was cut off each core and a I -in. diameter plug was taken from this section. Permeability to 5 percent by weight sodium chloride solution was determined and the large cores were

By R. T. Mishler

I WISH to express my keen appreciation of the article on the above subject by Coe and Clevenger.1 It has been doubly interesting to me, for the reason that the experience recorded and the principles evolved practically parallel the results of similar investigations made by myself and others at The Lucky Tiger Mine, El Tigre, Sonora, Mex. An outline of the work at El Tigre may aid in confirming the principles expressed by Coe and Clevenger. El Tigre has the unenviable distinction of possessing a slime with a much lower settling rate than any recorded in the article discussed. Under most favorable conditions the settling rate is about one-third that reported for the Liberty Bell mill, and one-tenth that reported for the Nipissing, Golden Cycle, and Presidio mills. This slow settling characteristic of Tigre ore has necessitated careful investigation of settling phenomena throughout the various evolutions of the plant. PREVIOUS SETTLING INVESTIGATION AT TIGRE During construction work at the mill, the Metallurgical Engineer in charge, D. L. H. Forbes, ran a series of experiments on settling. His tests proved that deep settling tanks were not ordinarily necessary. The use of tanks 2 or 3 ft. in depth was suggested.2 Later experiments demonstrated that the following principles of settling applied to Tigre pulp.3 1. In settling dilute pulp, settling rates are independent of pulp depth. 2. In settling thick pulp, settling rates are approximately proportional to pulp depth.4

Jan 3, 1917

By E. T. Dumble

(Cleveland Meeting, October, 1912.) FOR many years there have been occasional reports of the discovery of gold from a belt of the coast country of Texas which is underlain by deposits belonging to the lower Eocene. For the most part they have been treated as newspaper reports and no examination or record of them has been made. Among such, it may be mentioned that in 1896 there was a flurry over reported gold-discoveries -west of Luling and elsewhere in this belt, and in 1903 some prospect-shafts were sunk on the Gonzales branch of the Galveston, Houston & San Antonio railway, 3 miles below Harwood. During 1912, further discoveries have again brought the matter to our attention, and it may be of interest to record the facts as we have found them. Some years ago specimens were sent me, which were said to have been taken from certain beds on Gazley creek, and concentrated by washing in it rocker. In them were several particles of gold sufficiently large to be visible to the eye. Under the microscope they showed to be, with few, exceptions, sharp cornered, and not rounded as is usual with placer-gold. They were not filings, however, but their sharpness seemed rather to be due to a recent freeing from their matrix. One or two grains were rusty, and one copper-hued, but the most of them were tolerably bright. On examining the material of the samples small grains or fragments were found, of a yellowish brown color, which seemed to be of a finely-granular structure-possibly a sandstone. In these fragments I found particles of gold, one of them being large enough to be visible without a lens. Gazley creek empties into the Colorado river just north of Smithville, and for a few miles north of that place its banks show, beneath the deposits of more recent materials, the sands and clays of the Lignitic division of the Eocene, with lignite, shells of iron, etc.

Oct 1, 1912

By R. E. Ogilvie, E. T. Peters

The X-ray Kossel-line method has been used preaioz~sly for measuring lattice parameters to accuracies of 1 part in 100,000.5 A second application of this method is described for determining the crystallographic orientation of a randomly positioned single-crysta1 spherical volume that can he as small as 50 µ in diameter, within accuracy limits of ±1/2 deg. The theory, experimental procedure, and interpretation of Kossel-line patterns and an experimenta1 verification of the predicted orientation relationship of the cph k and fee a Cu-Si phases are presented. This orientation relationship can be described as (111)a, (00.1)k; [110]a [11.0]k. In addition, the lattice parameter of the a phase was found to he a. = 3.62154 ± 0.00014Å. The Kossel-line method when used in conjunction with electron microanalysis is shown to he capable of providing a complete chemical and structural analysis of a given crystal. THE most easily accomplished methods for determining the orientation of a single crystal are variations of the Laue X-ray diffraction method. Although certain materials can be oriented to within ± 1 deg accuracy by observation of exterior macroscopic features, such as etch pits, cleavage faces, or growth features, the Laue method is generally preferred for routine laboratory application. Both back-reflection and transmission patterns are coordinated by appropriate reference charts and are plotted in terms of reflection plane poles (normals) on a stereographic projection. Orientation is deduced by relating the pole distribution (which is fixed by the crystallographic symmetry of the specimen) to two specified external reference directions. The Laue method has several limitations. 1) Orientation can rarely be determined to better than ±l deg accuracy. Principal errors involve inaccuracy in specimen-to-film distance, measurement confidence of individual Laue spots, and stereographic plotting. 2) Because of the indeterminacy of the X-ray wave length diffracted to a given spot, it is not possible to determine supplementary crystallographic data, such as interplanar spacings and lattice parameters. 3) The method is generally limited to specimens of cubic symmetry or to specimens of high symmetry and known structure. 4) The relatively large cross-sectional area of the incident X-ray beam generally precludes the measurement of relative grain orientation in a polycrystalline material.* _____ Several of these limitations can be overcome by application of the Kossel-line method, which has been previously employed for precision lattice-parameter determinations.'-= For this method, a point source of divergent monochromatic X-rays is generated within the crystal by means of an incident electron beam. The divergent X-rays which fulfill the Bragg law are diffracted by the specimen and are recorded on a film placed either in transmission or back reflection. Analysis of the film yields a direct measurement of orientation and lattice-spacing values to an accuracy of ±1/2 pct. As analyses can be obtained from spherical specimen volumes as small as 50 µ in diameter, the method provides a means for structural analysis of second-phase or impurity precipitates within a given matrix. The primary limitation of the Kossel-line method is the requirement for an electron microanalyzer or similar apparatus capable of producing a finely focused electron beam. This paper is designed to present the theory, experimental procedure, and geometrical interpretation of Kossel patterns. The experimentally determined orientation relationship between the k and a phases occurring in the Cu-Si system and a precision measurement of the a lattice parameter are presented as a practical application of the method. THEORY OF KOSSEL LINES Divergent X-ray beam photography utilizes an effective point source of characteristic X-rays which, when diffracted from a single crystal, form numerous diffraction and absorption cones that are recorded on film.7 The cones generated from a source lying within the crystal are called Kossel lines.' Although the X-ray scattering from a divergent point source contained within a crystal is described in terms of Laue dynamical theory,9 the directions of the diffracted spectra can be ade-

Jan 1, 1965

By Albert J. Phillips

LEAD is an inexpensive metal produced and consumed in large quantities with certain chemical and physical properties that permit handling the molten metal in bulk. These properties are its low melting point, resistance to oxidation, and its negligible solvent action on iron and steel. Thus, lead is almost always melted in large iron or steel kettles, heated from beneath, and is seldom melted in either directly or indirectly fired furnaces or electric induction or arc furnaces. Even with a modest operation a kettle holding 2 or 3 tons is employed, and the size will range up to 215 tons in the large lead refineries. The methods of handling tin and its alloys are essentially the same as for lead because of the similarity in melting point and resistance to oxidation, although because of the cost of the metal the scale is more modest. In melting lead and its alloys preliminary to a casting operation it is seldom that the melting unit is completely drained of its contents. The usual procedure is to continuously charge solid metal and continuously remove small amounts of liquid metal, so that the kettle is maintained essentially full at all times. For type metals, linotype machines usually employ automatic means of adding the solid alloy to the melting pot in proportion to the removal of the liquid metal in casting slugs of type. In the casting of grids for storage batteries, frequently automatic means of charging solid metal in direct proportion to the consumption of liquid metal in the casting is used. In the manufacture of bearing alloys, new alloy is charged in direct proportion to the consumption of metal in the bearings being cast, so that at no time does the level of the metal in the melting pot lower to any great extent. Even in the manufacture of bulky commodities such as pipe, cable. sheathing, and slabs for rolled sheet, it is the practice to employ a melting kettle of several times the capacity of the casting being made. A substantial level of liquid metal in the melting kettle is thus maintained even after the casting is poured and the original metal level is quickly restored by promptly charging new metal, even though there is no immediate need to proceed with additional casting. This procedure is permissible because the amount of fuel consumed in keeping the lead molten and immediately available for use is negligibly small and the cost is more than offset by the convenience. However, this convenient procedure necessitates study and control of certain properties of lead and tin alloys that are not of serious consequence in most other alloys and for that reason are not well known. These properties are "drossing rates" and "melting segregation." DROSSING RATE Users of lead long ago observed that the rate of dross formation on the surface of the lead in their kettles or pots varied greatly from time to time. This was particularly common in places where both antimonial lead alloys and commercially pure lead were being handled.

Jan 1, 1946

W. G. MATTESON, Houston, Tex.-I think that Mr. Powers has given us some very valuable information on the Healdton field, which is of material interest in view of the fact that the Healdton field has passed Cushing in the point of production, and if not leading, stands second only to the new El Dorado field in the point of production of the oil-in this country. Mr. Powers says that the deepest producing sand at Healdton is 1860 ft. Within the last 3 or. 4 months they have drilled to 2700 ft. there and found a sand which is producing very high-grade oil, if I remember correctly, about 42 gravity. Another very important point brought out by Mr. Powers is the fact that the Pennsylvanian beds and the Permian beds are conformable according to his interpretation. He seems to have based his interpretation upon the gathering of a number of well logs and a very careful study of them, but it seems to me the information furnished by the, well logs is really insufficient to justify such an important conclusion. In the first place, the difficulty of interpreting the line of demarcation between the Permian "Red Beds" of Oklahoma and the top of the Pennsylvanian is apparent, for the reason that sometimes the uppermost Pennsylvanian formation has a reddish phase and the line of demarcation is not very sharp.

Jan 4, 1918

By Guy R. Johnson

In working brown iron-ore mines on the system employed at Longdale, namely, stoping from the top down, the usual procedure is to drive a succession of upraises from the lowest adit to the highest, or to the top of the deposit, as the case may be. These up-raises are usually driven 120 feet apart., along the strike of the vein,. As the work goes on, they are connected by levels, 10 feet spa* (vertically), and then serve as chutes. A transit is useless in surveying these chutes, and the writer has for several years made use of a hanging compass. The method of using this instrument, described in a former paper (Trans., xx.,.105), embracing as it does the use of a cord and several strips. of wood,

Jan 1, 1894

By Vaughn Moyer

A method for incorporating well drawdown effect into reservoir calculations is presented in detail, together with examples of its use for widely divergent conditions that could be normally encountered in oil reservoir sands. Tentative conclusions as to the effect such factors as permeability, producing interval, well spacing, or well damage caused by completion or repair practice could have upon economic ultimate recovery are reached. It is carefully pointed out that the conclusions reached are subject to limitations indicated in the text, and placed upon all calculations made in the paper. Introduction Papers have been presentedl-3 in which theoretical depletion histories for reservoirs under equilibrium conditions and no appreciable well-bore drawdown pressure are determined. However, except for a limited number of cases, appreciable drawdown Pressures in a well bore exist, and Pressure and saturation gradients consequently vary throughout a reservoir. This Paper is an attempt to incorporate well-pressure drawdown into reservoir history, and to analyze certain factors, such as those involving recovery, well spacing, and productivity index, from the standpoint of permeability and drainage radius. BY incorporation of drawdown into reservoir history, it is believed that theoretical considerations will more closely approxi- mate actual reservoir behavior experienced in an oil field. For purposes of simplification, a solution gas-drive type field1 without primary gas cap, has been selected. Basic Data and Assumptions Details of equilibrium saturation conditions for no drawdown production for various pressures in a reservoir are deter-minable by methods described by several are permitting the construction of a curve of oil saturation vs Pressure for any selected combination of initial interstitial water and hydrocarbon saturation (Fig I). This curve is then a description of equilibrium saturation conditions at any given pressure in a reservoir. Developing the above, details of saturation and flow permeability may thus be determined for any increment or portion of a well drainage area or reservoir. In this manner the effect of pressure differential (drawdown) may be incorporated into reservoir and well drainage considerations. It is pointed out that this method thus makes use of no-drawdown equilibrium production data, superimposing a draw-hwn effect upon them. It also assumes that net flow conditions in any considered increment of reservoir are not materially altered by the entrance of fluids from other increments into them, but approach equilibrium for the existing pressure and saturation (i.e., each increment behaves in more or less independent fashion, dependent largely upon the equilibrium considerations mentioned above)

Jan 1, 1948

By Vaughn Moyer

A method for incorporating well drawdown effect into reservoir calculations is presented in detail, together with examples of its use for widely divergent conditions that could be normally encountered in oil reservoir sands. Tentative conclusions as to the effect such factors as permeability, producing interval, well spacing, or well damage caused by completion or repair practice could have upon economic ultimate recovery are reached. It is carefully pointed out that the conclusions reached are subject to limitations indicated in the text, and placed upon all calculations made in the paper. Introduction Papers have been presentedl-3 in which theoretical depletion histories for reservoirs under equilibrium conditions and no appreciable well-bore drawdown pressure are determined. However, except for a limited number of cases, appreciable drawdown Pressures in a well bore exist, and Pressure and saturation gradients consequently vary throughout a reservoir. This Paper is an attempt to incorporate well-pressure drawdown into reservoir history, and to analyze certain factors, such as those involving recovery, well spacing, and productivity index, from the standpoint of permeability and drainage radius. BY incorporation of drawdown into reservoir history, it is believed that theoretical considerations will more closely approxi- mate actual reservoir behavior experienced in an oil field. For purposes of simplification, a solution gas-drive type field1 without primary gas cap, has been selected. Basic Data and Assumptions Details of equilibrium saturation conditions for no drawdown production for various pressures in a reservoir are deter-minable by methods described by several are permitting the construction of a curve of oil saturation vs Pressure for any selected combination of initial interstitial water and hydrocarbon saturation (Fig I). This curve is then a description of equilibrium saturation conditions at any given pressure in a reservoir. Developing the above, details of saturation and flow permeability may thus be determined for any increment or portion of a well drainage area or reservoir. In this manner the effect of pressure differential (drawdown) may be incorporated into reservoir and well drainage considerations. It is pointed out that this method thus makes use of no-drawdown equilibrium production data, superimposing a draw-hwn effect upon them. It also assumes that net flow conditions in any considered increment of reservoir are not materially altered by the entrance of fluids from other increments into them, but approach equilibrium for the existing pressure and saturation (i.e., each increment behaves in more or less independent fashion, dependent largely upon the equilibrium considerations mentioned above)

Jan 1, 1948

By Tom Westgarth

As papers are placed before you upon large gas-engines in Belgium and Germany, it was considered that some information should be given upon the same subject in Great Britain. I therefore agreed to compile these notes, which I have made very short in view of the somewhat full nature of the other papers presented to this meeting, and considering the complete nature of the many publications which have been made recently upon the subject of large gas-engines. I give below Tables I. to VI., showing the number and particulars of large gas-engines which have been built or are building by British makers, and in view of the growing size of gas-engines I have concluded that engines less than 500 h.p. cannot now be included in the category of large gas-engines, and therefore I have not considered engines under that power.

Nov 1, 1906

By Earl Hunner

IT is common knowledge that the iron orebodies of the Mesabi range lie nearly horizontal and are of trough or blanket-like types. These orebodies are from a few feet to several hundred feet thick and vary from a few acres in extent to the size of the largest one, at Hibbing, Minn., which is over 1 mile wide and 3 miles long. They are covered with sand, boulder and clay overburden and occasionally, shallow depths of ledge material, varying in total depth from about 20 to 200 ft. Large areas are not capped with overlying ledge material; the top of the ore lies directly underneath the surface material. Because of the comparatively great tonnage of ore, open-pit mining has made tremendous strides since the first open-pit ore was shipped from this range by the Merritt brothers, from the Mountain iron mine in October, 1892, and along with the great development of open-pit mining on the Mesabi range has gone a tremendous change in the character of equipment used.

Jan 1, 1930

By AIME AIME

. COUNCIL.* PRESIDENT OF THE COUNCIL. D. W. BRUNTON DENVER, COLO. (Term expires February, 1911.) VICE-PRESIDENTS OF THE COUNCIL. W. C. RALSTON SAN FRANCISCO, CAL. W. L. SAUNDERS : NEW YORK, N. Y. H. V. WINCHELL ST. PAUL, MINN. (Term expires February, 1911.) BENJAMIN B. LAWRENCE NEW YORK, N. Y. JOSEPH W. RICHARDS SOUTH BETHLEHEM, PA. ALBERT SAUVEUR CAMBRIDGE, MASS. (Term expires February, 1912.)

Apr 1, 1910

By AIME AIME

COUNCIL PRESIDENT OF THE COUNCIL. D. W. BRUNTON DENVER, COLO. (Term expires February, 1911.) VICE-PRESIDENTS OF THE COUNCIL. W. C. RALSTON SAN FRANCISCO, CAL. W. L. SAUNDERS NEW YORK, N. Y. H. V. WINCHELL ST. PAUL, MINN. (Term expires February, 1911.) BENJAMIN B. LAWRENCE NEW YORK, N. Y. JOSEPH W. RICHARDS SOUTH BETHLEHEM, PA. ALBERT SAUVEUR CAMBRIDGE, MASS. (Term expires February, 1912.)

Mar 1, 1910

By AIME AIME

PRESIDENT OF THE COUNCIL. D. W. BRUNTON DENVER, COLO. (Term expires February, 1911.) VICE-PRESIDENTS OF THE COUNCIL. W. C. RALSTON SAN FRANCISCO, CAL. W. L. SAUNDERS NEW YORK, N. Y. H. V. WINCHELL MINNEAPOLIS, MINN. (Term expires February, 1911.) BENJAMIN B. LAWRENCE NEW YORK, N. Y. JOSEPH W. RICHARDS SOUTH BETHLEHEM, PA. ALBERT SAUVEUR CAMBRIDGE, MASS. (Term expires February, 1912.)

Nov 1, 1910

By AIME AIME

COUNCIL.* PRESIDENT OF THE COUNCIL. D. W. BRUNTON DENVER, COLO. (Term expires February, 1910.) VICE-PRESIDENTS OF THE COUNCIL. J. PARKE CHANNING NEW YORK, N. Y. FREDERICK W. DENTON PAINESDALE, MICH. JOHN B. FARISH DENVER, COLO. (Term expires February, 1910.) W. C. RALSTON..: SAN FRANCISCO, CAL. W. L. SAUNDERS NEW YORK, N. Y. H. V. WINCHELL ST. PAUL, MINN. (Term expires February, 1911.)

Jun 1, 1909

By AIME AIME

COUNCIL.* PRESIDENT OF THE COUNCIL. D. W. BRUNTON DENVER, COLO. (Term expires February, 1910.) VICE-PRESIDENTS OF THE COUNCIL. J. PARKE CHANNING NEW YORK, N. Y. FREDERICK W. DENTON PAINESDALE, MICH. JOHN B. FARISH DENVER, COLO. (Term expires February, 1910.) W. C. RALSTON SAN FRANCISCO, CAL. W. L. SAUNDERS NEW YORK, N. Y. H. V. WINCHELL ST. PAUL, MINN. (Term expires February, 1911.)

Mar 1, 1909

By AIME AIME

COUNCIL.* PRESIDENT OF THE COUNCIL. D. W. BRUNTON DENVER, COLO. (Term expires February, 1910.) . VICE-PRESIDENTS OF THE COUNCIL. J. PARKE CHANNING NEW TORE, N. Y. FREDERICK W. DENTON PAINESDALE, MICH. JOHN B. FARISH DENVER, COLO. (Term expires February, 1910.) W. C. RALSTON SAN FRANCISCO, CAL. IV. L. SAUNDERS NEW TORE, N. Y. H. V. WIINCHELL ST. PAUL, MINN. (Term expires February, 1911.)

May 1, 1909

By H. H. Kellogg, T. R. Ingraham

Three anhydrous zinc sulfates have been identified. They are: ZnSO,(a), stable below 1007°K; ZnS04(/3), stable above 1007OK; and ZnO.ZZnSO,. The decomposition pressure of each sulfate has been measured and the following relations calculated from the results: The measured data have been combined with the known themzodynamic properties of ZnS, ZnO, Zn, SO,, and SO, to yield univariant and bivariant phase diagrams for the system Zn-S-0. The application of these diagrams to problems of roasting zinc concentrates is discussed. PRESENT knowledge of the equilibrium chemistry of the system Zn-S:O, so essential to scientific control of zinc-blende roasting, is deficient in several respects. A basic sulfate of zinc has been reported by many investigators, but its composition is in doubt and its thermodynamic properties have not been measured. Our scanty knowledge of the properties of the normal sulfate at roasting temperatures is based on old and inexact studies. A crystal transformation in the normal sulfate, involving a sizable heat effect, has been noted by several investigators but has never been quantified. The studies reported herein were designed to fill these gaps in knowledge and to make possible a reasonably complete thermodynamic description of the system Zn-S-0 at roasting temperatures. The results make possible a far more exact understanding of zinc roasting chemistry than was hitherto possible. EXPERIMENTAL The principal experimental technique employed was the measurement of the total gas pressure developed from decomposition of either ZnSO, or ZnO2ZnS0, in a closed system. The apparatus employed was essentially the same as that described by Warner and lngrahaml and Flengas and tngraham.' The unusual feature is a flexible Pyrex bellows used to separate the reaction gas mixture (S03, SOz, and 02) from the mercury in the manometer and thus prevent corrosion of the mercury by SO3. The bellows operates without evidence of hysteresis and, barring accidents, may be used for several months. The response of the bellows varies from manometer to manometer, but is generally of the order of 0.6-cm displacement for a l-cm change in pressure. The response for all manometers has been linear over the range 0 to 1 atm. To prevent condensation and polymerization of sulfur trioxide, the bellows-manometer was maintained at 100.0" * 0.5" by a circulating bath of silicone oil. The connecting tubing between the manometer and the furnace was maintained at 100.0" * 0.2"* also, with a stirred air bath. The open end of the manometer was connected with a chamber which was maintained at a known pressure. The pressure could be varied so that readings of the height of the mercury column, measured with a cathetometer, could be made with both rising and falling mercury column. By using the average of the readings, any error due to sticking of the mercury column was minimized. The sample was placed in a 2-in.-long platinum boat formed into the shape of a half-cylinder. The sample was prepared as a fine powder and pressed against the inner wall of the platinum boat. A silica thermocouple well, covered with a platinum sleeve, was placed lengthwise along the center of the boat. The temperature of the sample was read on a calibrated Pt-10 pct Rh theirnocouple. The temperature profile of the furnace was constant within ± 0.2 C over the length of furnace occupied by the sample. The horizontal furnace used to contain the sample and the quartz reaction tube was electrically heated, with the control thermocouple placed 1/4 in. from the windings. A Brown Pyro-O-Vane temperature controller with a 3-sec response time was used to maintain the furnace temperature. Before beginning a run, the apparatus, including the bellows manometer, was thoroughly washed in sib with acid and distilled water to remove any

Jan 1, 1963

By N. J. Grant, B. C. Giessen, Paul Predecki

ALLOYS of gold, silver, and aluminum with elements of the groups BII, BIII, BIV, and BV were prepared by a rapid quenching technique (splat) and were examined by X-ray diffraction. Five new intermediate phases were found and will be described briefly herein. For the gold and silver systems, the concentration ranges having an electron/atom ratio e/a of 1.4 to 1.5 ("3/2 Hume-Rothery phases") were studied primarily. Master alloys were prepared from high-purity metals (99.9+ pct or better) by melting either in evacuated fused silica capsules or by nonconsum-able-electrode arc melting in an argon atmosphere. Small pieces, 20 to 50 mg, of each alloy were blast-atomized to form a splat, by a technique similar to that described by Duwez and Willens.1 The technique used for this study is described in detail in Ref. 2; it utilizes a resistance-heated graphite crucible with a small hole at the bottom, directed toward a metal substrate or quenching plate. The prepared alloy rests over the fine hole, through which it is expelled by an explosion shock wave in the form of fine droplets (1 to 50 µ) of molten metal onto a copper or silver substrate, which is maintained at about -190°C. The resulting very high cooling rates (see Ref. 2 for quantitative measurements) can prevent the process of nuclea-tion and growth in many instances, resulting in the formation of metastable phases. The splat particles were transferred to a GE-XRD5 diffractometer and maintained at -190°C, where they were examined with CuKa radiation. The samples were then allowed to warm to room temperature or were heated to higher temperatures until the equilibrium structures formed. Of fifteen alloy systems considered, nonequi-librium structures were encountered in six; these are described below and summarized in Table I. In the system Au-Sb a metastable £ phase (A3 type, hcp, a = 2.898 + 0.002A; c = 4.731 * 0.004A; c/a = 1.633) was found in the concentration range Au + 13 to 15 at. pct Sb. This phase is isomorphous with the stable phases in the systems Au-Cd, Au-In, and Au-Sn, all at an average e/a ratio of 1.4 to 1.5. The concentration range of one-phase metastable was deduced from the small amounts of supersaturated gold solid-solution phase present in the splat product. It was found that ? could also be retained by splatting onto a substrate held at room temperature: however, decomposed into the equilibrium phases Au + AuSb2 after heating to 200°C for 1/2 hr, or on holding the powdered splatted alloy at 20°C for several months. Calorimetric measurements will be made in an attempt to decide the question whether ? is metastable at all temperatures or whether it is a stable phase at low temperatures. There is evidence that another phase, possibly also close-packed but with a different stacking sequence, can be obtained by rapid quenching of alloys with a different antimony content. Klement, Willens, and Duwez3 reported the existence of an amorphous phase on quenching Au-Si alloys (25 at. pct Si) to - 196°C. They found that on heating to room temperature another phase of unknown crystal structure was formed. This was confirmed (see Table I); however, the new crystalline phase, designated as ?, could also be formed simply by rapid quenching to room temperature, and even was found to exist already in the as-cast Au + 20 at. pct Si alloy. It was found that ? decomposed into Au + Si on the specimen surface at room temperature. This behavior, and the question whether or not there is an equilibrium-temperature region for ?, have not yet been resolved. It is probable that ? (Au + 20 to 21 at. pct Si) is cubic of the -brass type (D81-3) with a = 9.60, + 0.01A and N = 52 atoms per cell [compare 6 (CU-Sn)4]. Except for two very weak lines, the powder pattern of about thirty lines could be indexed on this basis; however, a determination of the atom positions has not yet been attempted. For Au-Ge the C phase was observed at about 21 at. pct Ge as reported by Luo et at.5 Lattice parameters a = 2.876A, c = 4.73,A, c/a = 1.64 were found. In the Au-Pb system, formation of a ? phase was not observed, but in the lead-rich region at 75 at. pct Pb, broad peaks belonging to an amorphous phase were found. The maximum diffracted intensity occurred at 28 = 32.4 deg which is about 1 deg larger than the position of the (111) line of lead (Cuka). For Ag-Pb, an amorphous phase analogous to the one found in the Au-Pb system was observed; this metastable phase exists probably at about 75 at. pct Pb. Since no lead-rich alloys were tested, all alloys consisted of silver + amorphous phase at -190°C. In A1-Ge alloys, line-rich and complex powder patterns were obtained at about 30 at. pct Ge; they bear similarities to those of aluminum and germanium, but are of lower symmetry; the existence of more than one intermediate phase is possible. The authors are grateful to the Kennecott Copper Corp. for Fellowship support, and ARPA (Contract

Jan 1, 1965

By Lawrence Addicks

AT the San Francisco meeting of the Institute last year, I presented, through the courtesy of Dr. James Douglas; some results of experiments on the roasting and leaching of concentrator tailings. After it became apparent that flotation rather than leaching was clearly the better method of handling the particular problem under consideration, before dismantling the experimental equipment, some data were secured on roasting and leaching the concentrate itself in competition with smelting. Some of the results obtained are given in the following paper and they a re of particular interest at this time in. view of the large quantities of flotation concentrates with their somewhat difficult smelting characteristics now being produced. A complete wet process? consists of roasting and leaching the calcines in dilute sulphuric acid produced from the roaster gases, roasting the residue with salt and leaching with dilute tower liquors (the well-known Longmaid-Henderson process) and recovering the copper, silver and gold by cementation or electrolysis or a combination of both. It is evident, however, that the residue from the first leaching, carrying about 20 per cent. of the copper and all of the silver and gold, can be smelted if preferable. In considering the application of the scheme to individual cases, it must be remembered that freight plays a. large part in any reduction process wherein smelting is not conducted at the, mouth of the mine, and that it is not practicable today to build small smelting plants for individual operations. The experiments may be grouped under four main heads: Roasting, leaching, chloridizing residue, and recovery of copper from solutions. The products of two concentrators were used: The Nacozari concentrates were the product of a large modern mill not using flotation, the copper mineral being largely chalcopyrite; and the Tyrone concentrates, the product of an experimental mill including flotation, the copper mineral being chiefly chalcocite. Typical analyses would be as follows:

Jan 9, 1916