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By Harold Margolin

The Ti-Al system certainly merits the investigative attention it has been receiving and this latest contribution by Blackburn is therefore to be welcomed. The titanium-rich end of the phase diagram shown here, as well as the diagram by crossley,17 Clark et a1.,18 and Tsujimoto and Adachi,29 reveal no other intermediate phase than Ti3A1, although a previous work by Ence and Margolin20 had reported an additional intermediate phase. Since then, Buerger Precession pictures of single crystals of 10.5, 11.5, and 12.5 wt pct A1 were made at New York university21 and the extinctions were found to be typical of a D6h a Ti structure. Some superlat-tice spots and/or streaks suggesting the presence of an Mg3Cd structure, i.e., Ti3Al, were also found. Since these specimens had been quenched from the y region20 and had revealed a Ti, it was concludedz1 that y does not exist and the structures interpreted as m + y could not be so considered. The absence of normal two-phase behavior in these structures had been indicated in the paper. Accordingly, the two-phase region y + 6 becomes a + Ti3Al and there is some agreement between the results of Blackburn and of Ence and Margolin20 as to both shape and existence above 900°C of an a + Ti3Al field. Crossley 17 proposed that Ti3Al is a line compound which decomposes congruently at 900°C. It is difficult to discount entirely the fact that clear two-phase structures, varying in amount with position in the two-phase field, could be detected above 900°C by Ence and Margolin.20 Precipitation during quenching could not have been so regular and the twin-phase syndrome17 does not apply. The heat treatment and quenching technique was essentially the same as was used by Crossley, whereas Blackburn, who used a rapid quenching procedure, also showed a two-phase a + Ti3A1 field above 900°C. If the two-phase field exists above 900° C, it is easy to picture a two-phase field which could account for the data of Crossley below 900°C without invoking a line compound existence of Ti3A1. All that would be necessary would be an 0 + Ti3Al/Ti3Al boundary which curved sharply to higher aluminum contents below 900° C. It is clear that the controversy must be solved by techniques which obtain data at elevated temperatures without quenching. It is conceivable that the difference in width of the a + Ti3N fields reported by Blackburn and by Ence and Margolin is due to the longer annealing times used by the latter investigators. The criterion for establishment of equilibrium in our work20 was the

Jan 1, 1969

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

The basic structural unit of all silicate minerals is a tetrahedron with a silicon atom at the center and four oxygen atoms at the corners. The oxygen-silicon distance is about 1.6 & and the oxygen-oxygen distance about 2.6 &. The different types of oxygen-silicon frameworks in the various silicates are based entirely on the combinations of the tetra-hedral oxygen-silicon groups through sharing of oxygen atoms. In recent years, infrared spectroscopy has permitted estimation of the ratio of the ionic character of the oxygen-silicon bond to be a few times that of the oxygen-carbon bond and the ratio of electro-negativity of the two bonds has also substantiated this finding. On this basis, it is generally accepted that the oxygen-silicon bond is the strongest one occurring in silicate minerals. As the oxygen-silicon ratio increases from quartz to the olivines, a greater percentage of the oxygen bonding power is available for bonding to cations other than silicon. Hence, with an increasing oxygen-silicon ratio, there is increasing oxygen-to-metal bonding. Upon the fracturing of a silicate mineral crystal, the oxygen-metal bond, which is almost entirely ionic in character, should break more easily than the stronger oxygen-silicon bond, resulting in a greater number of unsatisfied negative forces on the surface. If, then the mineral is immersed in a liquid containing hydrogen ions, these negative forces should tend to be neutralized by hydrogen ions from solution, resulting in a change of the pH of the solution. An increase in the degree of adsorption of hydrogen ions is to be expected as the oxygen-silicon ratio in the crystal structure increases. This study attempted to correlate the oxygen-silicon ratio for various representative silicate minerals to the adsorption of hydrogen ions. Experiments to determine the effect of surface area on this adsorption and to investigate the effect of surface iron were also conducted. It is believed that such studies of the surface properties of silicate minerals will supply pertinent information about their behavior in froth flotation systems. EXPERIMENTAL PROCEDURE Ion Exchange: Carefully selected, hand-picked samples of the minerals investigated were dry-crushed in a ceramic ball mill and sieved to obtain a minus 100 plus 200-mesh sample. The sized samples were then run through the electro-magnetic separator to remove any iron-bearing particles. A 10-g sample of each mineral was placed in 100 ml of freshly deionized water previously adjusted to a pH of 3.50 with HCl. The beaker containing the sample and the water was placed under a bell jar from which the air was displaced at once by nitrogen gas from a tank. All experiments were carried out in a nitrogen atmosphere. The sample and solution were stirred gently but continuously during the entire experiment, the stirring speed being kept about the same for all runs. Changes in pH were followed with a Beckman Zeromatic pH meter and recorded on a

Jan 1, 1967

By L. Albert, A. M. Cameron, J. W. Gullick

International Nickel has 15 operating mines in Canada, and. 3 mines which are being maintained on a standby basis. Annual production is about 20 million dry short tons of ore, most of which is from underground mines, the remainder from open pit mines. Although some of the underground mines are served by ramps for trackless vehicles, most men, materials and ore are hoisted in vertical shafts. In addition to shafts and raises for ventilation and service purposes which are not equipped with hoisting plants, there are now 28 vertical shafts at Inco mines served by 47 hoists. Of these, 22 shafts and 36 hoists are located in the Sudbury District of Ontario, one shaft and two hoists are at the Shebandowan mine in Western Ontario, and 5 shafts with 9 hoists are located near Thompson, Manitoba. This paper describes the components of Inco hoisting plants-which have been applied at different times and under different conditions, and indicates the rationale for the various designs. Some engineering and maintenance practices, considered advantageous, are also described. MINE SHAFTS Many of the shafts sunk in the early days of the Sudbury District, on what are now Inco properties, were inclined shafts. Of the identifiable shafts sunk between 1885 and 1920, thirteen were inclined and at least four were vertical. Since 1920, thirty vertical and two inclined shafts have been sunk. All of the inclined shafts have been abandoned for hoisting purposes but the majority are still in use as service or ventilation ways. Shafts at Thompson- and Shebandowan are all vertical. The vertical shafts range from 2 or 3 compartment exploration and development shafts to 6 compartment shafts for ore, man and material hoisting. They vary in depth from 1,050 to 7,137 feet and in addition to hoisting compartments all contain manway and service compartments. Prior to 1948, unlined rectangular shafts with timber sets and guides were used. The rectangular cross-section was favoured since the rock is competent, the shape compatible with timber set framing, and since available shaft space could be used efficiently. Resistance to air flow was not of prime importance. Concrete linings were introduced for the first time at the Creighton No. 7 Shaft which was collared in 1948. All major shafts since that date have been concrete lined. Vertical set intervals were increased in steps, with the introduction of structural steel sets secured to the concrete linings. Whereas 7 foot set intervals were used with timber framing, this increased to 10 feet 6 inches with steel sets and more recently to 15 feet with steel and steel backed wood guides. With the advent of deeper shafts, or shafts which are expected to be deepened, the trend is to circular concrete lined shafts. The majority of shaft guides in service are of select Douglas Fir. This practice commenced as a component of timbered shaft design but continued as a

Jan 1, 1975

By Stanley C. Herold

TWENTY-FIVE years ago no distinction was made between water wells and oil wells except in the nature of the fluid produced. Water wells usually showed no decline in their rate of production; when oil wells showed decline something in the manner of handling them was considered wrong. Both water and oil were believed to be subject to the same physical laws in their underground movement toward the wells. Today a sharp distinction is made between them. Whereas water exists alone in the porous formations at depth, oil is usually accompanied by gas. This mixture does not behave as a liquid alone. It is a frothy, seething mass of foam which approaches and enters the wells. Different physical laws come into play. Twenty-five years ago attention was directed entirely to the well itself; today the well is accepted as a mere hole in the ground, a hole to be equipped properly for efficient service, yet without any value whatever unless it is backed up by a sufficiently prolific reservoir. Then, we were concerned with wells alone, 3000 ft. in depth; now commercial wells and their reservoirs are 10.000 ft. deep. Petroleum engineering concepts have necessarily therefore undergone a change in this last quarter century. What are they today?

Jan 1, 1937

By B. Blumenthal

THE present investigation was planned as a survey of the lead-rich portion of the ternary lead-antimony-silver system by thermal analysis. Since, however, a rigorous application of the conventional thermal analytical method is time consuming, an attempt was made to speed up the investigation by reducing the time required for a single thermal analysis. This was done by increasing the rate of cooling to 12° to 18°C. per minute, since such a rate does not permit even an approach to equilibrium conditions, the melt was stirred vigorously by a stirrer operating at the high rate of 665 r.p.m. This proved to be effective in obtaining cooling curves with distinct points of arrest and of excellent reproducibility, which satisfactorily compare with those obtained at a rate of 1" to 2°C. per min. with or without slow stirring (Fig. I). By this method the lead-rich end of the lead-alltimony system and a series of ternary alloys in sections parallel to the lead-antimony side of the ternary system were investigated and it was observed that the two branches of the liquidus curve of the binary alloys did not intersect at the euteotic temperature. An equivalent effect mas observed in the ternary system. The eutectic temperature of the binary lead-antimony system was found to be 252.0°C., which confirms the recent in- vestigation by Pellini and Rhines,1 who determined the eutectic temperature to be 2 51.5°C. The observation that the curves of primarY crystallization of the lead-antimony system do not intersect at the eutectic temperature was previously made by Dean.2 Dean explains the phenomeilon by assuming the existence of a compound Sb4pb. He felt that supercooling was not the cause of the phenomena because he was unable to influence them by inoculation. The X-ray investigation by Solomon and Morris-Jones,3 the metallographic investigations by Stead,4 Charpy,5 Gontermann,6 and Dean, Zickrick and Nix,7 and the numerous investigations of physical properties, definitely disprove the occurrence of any compound. The work of Dean was not confirmed by Broniewski and Sliwoski,8 whose experiments did not show any irregularity and who report a eutectic composition of 13 per cent antimony and a eutectic temperature Of 2500 to 252°C. at a rate Of coo1ing of about 6°C. Per min. Abell Redlich and Adler9 then report a eutectic composition of 12.1 per cent upon reviewing the previous publications and adding a few of their own cooling curves. In 1934 Quadrat and Jiriste10 found from careful analyses of the bottom portion of slowly cooled hypereutectic melts that the eutectic only 11 .4 to 11.5 per cent antimany. (Previous analyses by Stead4 .in 1891 gave 13 per cent.) Weaver,ll however, reported in 1935 that cooling cunres indi-

Jan 1, 1944

By B. Blumenthal

THE present investigation was planned as a survey of the lead-rich portion of the ternary lead-antimony-silver system by thermal analysis. Since, however, a rigorous application of the conventional thermal analytical method is time consuming, an attempt was made to speed up the investigation by reducing the time required for a single thermal analysis. This was done by increasing the rate of cooling to 12° to 18°C. per minute, since such a rate does not permit even an approach to equilibrium conditions, the melt was stirred vigorously by a stirrer operating at the high rate of 665 r.p.m. This proved to be effective in obtaining cooling curves with distinct points of arrest and of excellent reproducibility, which satisfactorily compare with those obtained at a rate of 1" to 2°C. per min. with or without slow stirring (Fig. I). By this method the lead-rich end of the lead-alltimony system and a series of ternary alloys in sections parallel to the lead-antimony side of the ternary system were investigated and it was observed that the two branches of the liquidus curve of the binary alloys did not intersect at the euteotic temperature. An equivalent effect mas observed in the ternary system. The eutectic temperature of the binary lead-antimony system was found to be 252.0°C., which confirms the recent in- vestigation by Pellini and Rhines,1 who determined the eutectic temperature to be 2 51.5°C. The observation that the curves of primarY crystallization of the lead-antimony system do not intersect at the eutectic temperature was previously made by Dean.2 Dean explains the phenomeilon by assuming the existence of a compound Sb4pb. He felt that supercooling was not the cause of the phenomena because he was unable to influence them by inoculation. The X-ray investigation by Solomon and Morris-Jones,3 the metallographic investigations by Stead,4 Charpy,5 Gontermann,6 and Dean, Zickrick and Nix,7 and the numerous investigations of physical properties, definitely disprove the occurrence of any compound. The work of Dean was not confirmed by Broniewski and Sliwoski,8 whose experiments did not show any irregularity and who report a eutectic composition of 13 per cent antimony and a eutectic temperature Of 2500 to 252°C. at a rate Of coo1ing of about 6°C. Per min. Abell Redlich and Adler9 then report a eutectic composition of 12.1 per cent upon reviewing the previous publications and adding a few of their own cooling curves. In 1934 Quadrat and Jiriste10 found from careful analyses of the bottom portion of slowly cooled hypereutectic melts that the eutectic only 11 .4 to 11.5 per cent antimany. (Previous analyses by Stead4 .in 1891 gave 13 per cent.) Weaver,ll however, reported in 1935 that cooling cunres indi-

Jan 1, 1944

By D. V. Carter, Dan C. Williams, John R. Coombs

Exploration was active in East and East Central Texas during 1944. Ten oil fields were discovered during the year, of which four show promise of development. The discovery wells of the Sand Flat and Tyler, South fields were drilled to a depth greater than 10,000 ft., and the latter field now produces from the Pettit at a depth of 9890 ft. The Sand Flat well was plugged back to the Paluxy. The other two fields are Glen Rose producers near 8000 ft. The Pickton field produces from the Bacon Lime and Winnsboro from the Rodessa section. The Eylau field, Bowie County, was significant as the first Smackover production in Texas. Magnolia drilled a test in the Concord field, which topped salt. The most extensive and significant development in the district was the Carthage gas-condensate field. It expanded from the 8000 acres of last year to an estimated 190,000 acres, or about 300 sq. miles, and is not defined as yet. The first oil production in the Carthage area was made from the Travis Peak in 1944 in the Rogers Lacy's Cameron Lumber Company well No. I, on the northwestern side of the field. The New Hope field, Franklin County, scored the largest number of completions during 1944 with 24, bringing its total number of wells to 27. Two more pays were opened and produced as dual completions with the older horizons. The Manziel field, Wood County, had 19 new wells added during the year, for a total of 29, while the Pittsburgh field, Camp County, reached a total of 23 wells by completing 14 new ones. Material shortages and drilling restrictions dropped the total number of producing wells completed in the district from 171 during 1943 to 141 for 1944. Abandonments increased from 531 during 1943 to 609 for 1944. Of this number, 479 were in the East Texas field. Subsidy payments had very little effect in the district and it was mostly a few of the old fault-line fields that had any wells to fall within the requirements for subsidy payments. The prices of crude oil remained constant in the district except for increases as a result of subsidy payments. Production and Probation Wartime demands called for increased allowables for many fields, consequently the condensate and oil production for 1944 increased to 190,016,180, which is up 6.9 per cent over 1943. The East Texas field, of course, remained the principal producer of the district, accounting for 134,768'499 bbl. during the year, or 71 per cent of the district total production of condensate and oil. The field topped its own 1943 production by 4.8 per cent and became the first field in the world to produce 2 billion barrels of oil. The Hawkins field remained the second largest oil producer in the district, with 13,317,088 bbl. for the year, a drop of 6.8 per cent from 1943, while Van field was third with 11,635,708 bbl. The

Jan 1, 1945

By B. A. Rogers, K. O. Stamm

BECAUSE it is the basis of the economically important operation of hardening steel by quenching, the A3 transformation in iron has been the subject of numerous investigations. Although the contributions to this subject are interesting, no general review will be given here. Readers who care to follow the matter further are referred to the comprehensive summary by Cleaves and Thompson,1 which covers the literature to about 1935. Their references to 53 papers on the subject suggest that further investigation is hardly justifiable. However, considerable interest has developed recently concerning the reversibility of the transformation. From thermodynamic considerations, the transition ought to occur at the same point on heating or cooling, if the change of temperature is sufficiently slow. Yet all of the earlier investigators found a difference of several degrees. Burgess and Crowe,2 who used thermal methods, obtained average temperatures of 912° for Ac3 and 900°C. for Ar3 on electrolytic iron. Their data indicate a considerable range of temperature over which the change occurs, both on heating and on cooling. Terry3 measured the susceptibility in the critical range and estimated from the steepest parts of his curves that Ac3 came at 9180 and Ar3 at 903°C. Ishiwara4 was one of the first investigators to report a shorter interval between the temperature of the change in the two directions. He measured the change of susceptibility of kaolin-coated samples of steel, in a hydrogen atmosphere, at rates of heating and cooling so low that about 3 or 4 hr. were required for the transformation to complete itself. His results show some variability between samples, but indicate that the difference between Ac3 and Ar3 is in the vicinity of 6°C. Roberts and Davey5 measured the space lattice in pure iron in the vicinity of 900°°C. and concluded that a change occurs reversibly between 907° ± 3° and 9100 ± 3°C., probably between 907° and 910°C. Wells, Ackley, and Mehl6 made dilatometric determinations of the Ac3 and Ar3 points in samples of hydrogen-treated carbonyl iron maintained under a vacuum. They used three rates of heating and cooling: 2°, '1/2°, and 1/8°C. per min. and found the spread between the two points decreased with low rates. At the slowest rate, the Ac3 transition occurred at 909° to 909.5°C. and the Ar3 change at 907°C. in three of the samples believed to contain the lowest percentages of alien elements. They concluded that if the rate of temperature change and the content of alien elements were low enough, the A3 transformation would be completely reversible at 909.5° ± I°C. The question of reversibility is an interesting one and when some iron with especially small percentages of alien elements became available the opportunity to conduct an investigation was welcomed. This iron was prepared by the Division of

Jan 1, 1941

By William B. Heroy

LOOKING back over the industrial and commercial progress of the United States during the last half century the outstanding influence has been the growth of the use of the fluid fuels, petroleum and natural gas. At the turn of the century these fuels supplied only 8 per cent of the energy requirements of the nation. Last year nearly 45 per cent of our heat and power supply were derived from these fuels. These figures are merely statistical reflections of the fundamental change in our national economy which has affected, in so many amazing ways, the life of this generation. The factors which have caused this change are still operative. The trend which has thus been established still continues and growth in the use of these fuels is, in all probability, still well below the peak, both for this country and for other parts of the world. Two great wars have not essentially changed this basic trend; if anything they have served to accelerate it. World War II did not alone increase our requirements for liquid fuels; it demonstrated the absolute essentially of petroleum resources to our national security. Petroleum is no longer just an important factor in our national standard of living; it is the most important single element in our national defence-

Jan 1, 1946

By John W. Crutchfield, Emil F. Bowers

This paper presents the initial results of a pressure maintenance by water return project in the Lower Pawelek reservoir of the Falls City Field, Karnes County, Southwest Texas. Production is from the Lower Wilcox section at an average depth of 6,030 ft on the downthrown side of a "down to the coast" fault. Of particular interest is that the reservoir oil is high gravity and low viscosity but far undersaturated with gas at the original reservoir pressure and temperature. The early pressure and production history indicated only a partial or limited water drive, and this fact, coupled with the characteristics of the reservoir fluid and artificial lifting problem.. made advisable the water injection program to maintain reservoir pressure. The paper includes a description of the reservoir and reservoir fluids, the pressure and production history, a description of the water injection facilities, and the results of reservoir calculations involving Hurst's unsteady state flow and the material balance equations for calculation of water influx and prediction of the pressure-production relationship at various rates of withdrawal. The reservoir calculations and initial field results indicate that reservoir pressures in excess of 85 per cent of original pressure can be maintained by control of water injection even at very high rates of production. INTRODUCTION The purpose of this paper is to report the initial results of a pressure maintenance by water return program in the Lower Pawelek reservoir, Falls City Field, Karnes County. Texas, and to calculate an empirical relationship between pressure and production in this limited or partial water drive reservoir. Location The Falls City Field (Fig. 1) is located two miles north of the town of Falls City in Karnes County, Texas, and is approximately 50 miles south-southeast of San Antonio on U. S. Highway 181. Discovery and Development The initial block of leases was taken after a surface geological survey identified a major east-west fault and closure on the south or downthrown section. The discovery well, Southern Minerals Corporation's Joe F. Bartosch 1; was completed at 4,650 ft in the Lower Bartosch sand in December, 1944. Drilling was continuous until December, 1946, and resulted in the discovery of 12 oil reservoirs between 4,600 and 6,050 ft in the Middle and Lower Wilcox formations. These are shown on the cross-section (Fig. 2). As of the current date there are 64 oil wells completed as follows: Southern Gulfshore Magnolia Minerals Oil Petroleum Reservoir Corp. Co. Corp. Total Upper Bartosch 0 0 0 0 Lower Bartosch 16 0 0 16 Shulze 7 0 1 8 Upper Faires 2 0 0 2 Lower Faires 4 0 0 4 Upper Moczygemba 0 0 0 0 Lower Moczygemha 2 0 0 2 Olinick 2 0 0 2 Upper Martinez 0 0 0 0 Lower Martinez 5 0 0 5 Upper Pawelek 0 0 1 Lower Pawelek 27 1 3 31 Total 65 2 4 71

Jan 1, 1950

By James F. Watson, Jack L. Christian

The austenite to martensite solid state phase transformation in the 300 series austenitic stainless steels was studied over the temperature range of 788° to -423°F. The primary variables controlling this transformation are temperature, plastic strain, and chernical composition. Consequently, temperature effects were studied by measurements at 78", -100°, -320°, ad -423°F; plastic strain was controlled by cold-rolling the alloys varying amounts between 40 and 80 pet; and chemical compositions were varied by using 301, 302, 304 ELC, and 310 stainless steel alloys which exhibit varying degrees of austenite stability. The martensite contents of various alloys were correlated with several mechanical properties including yield and ultimate tensile strength, elongation, and notched tensile strength (Kt = 6.3). The yield and tensite strengths generally increased with increasing martensite content, but ) no correlation was observed between elongation and martensite content. The notched/un-notched ratio (Kt = 6.3) at -423°F exhibited a maximun at about 65 pct martensite. Attempts to correlate austenite stability (as measured by the Ms temperature) with both martensite content, and incremental increases in martensite content resulting from tensile testing were generally unsuccessful because the variable of cold Work could not be separated. As a result, only a general correlation of these variables was obtained. A (111) pole figure of austenite in a cold-rolled 301 stainless steel mas prepared an attempt to further investigate directionality as exhibited by mechan- ical properties. Yield strength was correlated with this pole figure, but ultimate and notched tensile strengths were not. 1 HE literature contains a wide variety of references pertaining to the austenite to martensite solid state phase transformation in austenitic stainless steel, see references 1 through 18. Discussions of the crystallography and kinetics of this transformation are given in references 2, 7, 8, 'and 11, while further discussions of austenite stability and hardening mechanisms are given in references 1, 3, and 10. Two important processing variables involved in this reaction are the degree of cold work and the temperature at which cold work is performed, and the nature of these effects are outlined in references 4 and 12, and 15 and 16 respectively. The latter two references deal primarily with cold rolling conducted at subzero temperatures. The effect of chemical composition on the austenite to martensite reaction was treated in detail by Eichelman and Hull, and they determined an equation for the M, temperature of this type of steel which included the effects of nickel, chromium, carbon, nitrogen, silicon, and manganese.5 Previous studies have shown that austenitic stainless steels of AISI types 301, 302, 304ELC, 310, and 301-N exhibit mechanical properties between 78" and -423"~ that are microstructure dependent, and the dependence of this microstructure on chemistry, temperature, tensile stress, and prior deformation is in general accord with previous investigations which have measured the effects of each of these variables on structure, or more specifically, the austenite-to-martensite transformation.lg The behavior of fully stable alloys, such as ATST type 310, at cryogenic temperatures is

Jan 1, 1962

By J. A. Morgan, R. E. Lund, D. E. Warnes

The design, operation, and performance of an integrated pilot plant for recovering zinc and copper from a complex sulfide ore are described. Metallurqical processing comprised selective sulfate roasting in a fluid bed, leaching in a weak sulfuric acid solution, recovering copper by cementation with scrap iron, air oxidation to remove soluble iron, more-or-less conventional Purification for removal of impurities deleterious to zinc electrolysis, recovering zinc by electrolyzing solutions, and recycling spent electrolyte to the sulfating roaster. The effects of several feed preparation and roasting variables on the sulfation response of zinc, copper, and iron are set forth, together with the electrolyzing characteristics of the zinc solutions. SEVERAL years ago, St. Joseph Lead Co. undertook a research program to develop procedures for winning values from a complex ore. The deposit was a massive sulfide ore body containing upwards of 65 pct pyrite. Gangue, composed principally of quartz, calcite, dolomite, and alumina, comprised only 10 to 20 pct of the mineralized zones. Zinc, lead, and copper values were variable, but averaged about 6.7 pct Zn, 2.6 pct Pb, and 0.4 pct Cu. Early in the exploratory test work, it was established that the intimate physical association of the minerals in the ore made beneficiation by conventional flotation procedures difficult. Accordingly, in addition to a comprehensive program to investigate physical methods of ore beneficiation, a research program was established to develop a direct metallurgical method for processing the ore. After surveying a number of potential methods for recovery of both metal and sulfur values, effort was concentrated on the development of a sulfate roasting process. It is the pilot-plant development of the sulfate roasting-solution purification—electrolyzing procedures which forms the subject of the present paper. PREPILOT PLANT INVESTIGATIONS From a thermodynamic viewpoint, it is feasible to sulfate selectively a host of metals, including Zn, Cu, Pb, Cd, Ni, and Co, in an iron sulfide ore without sulfating iron. Of course, a number of conditions such as roasting temperature and gas composition must be controlled. In addition, as first disclosed by Hybinette,' an alkali metal salt is frequently beneficial in promoting the sulfation reactions. The application of fluid bed roasting to the sulfate roasting of nonferrous metals was pioneered by Stephens of Battelle Memorial Institute.' Subsequently, Falconbridge Nickel Mines, Ltd. developed an unique process for selectively sulfating and recovering nickel, copper, and cobalt from their nickeliferous pyrrhotite, which recently has been described in an excellent paper by Thornhill.3 One of the unique features of the Falconbridge process is that the feed is introduced into the fluidized roasting furnace in a manner such that the feed slurry is broken up into droplets and the droplets lose their moisture before contacting the surface of the fluidized bed. The dried droplets do not tend to cake or fuse, but rather remain as discrete agglomerates of concentrate particles and roast without significant degradation. St. Joseph, aware that Battelle Memorial Institute had participated in the development of the Falconbridge process, obtained permission from Falcon-

Jan 1, 1962

The Pinto Valley, Arizona, plant of Cities Service Company is one of the newest copper producers in the United States, having started production in 1975. It is located a few miles west of Miami, Arizona, on the site of the Castle Dome Mine, a World War II operation which was shut down and its mill later moved and renamed the Copper Cities plant. The Pinto Valley concentrator uses six 18 ft (5. 5 m) diameter by 21 ft (6.4 m) long, 4000 hp, single-stage ball mills, taking crushed ore from four 7 ft (2. 13 m) standard and eight 7 ft shorthead crushers. It has a design capacity of 40,000 stpd but has higher tonnage capability for an expanded concentrator. The copper porphyry-ore is mined by two 15 yd and one 20 yd shovels (11.5 and 15.3 cu m) and is transported to the primary crusher by 150-ton trucks. The dump pocket is relatively shallow (14 ft or 4. 27 m deep); and because of the width necessary for the 150-ton trucks, it was designed to use the ore itself instead of manganese steel as an abrasion- resistant lining, although a heavy steel cap protects the dump pocket top edge. The pocket has a capacity of 300 tons of ore. Water sprays under the dumping positions direct a fog toward the truck being dumped for excellent dust control. Breaking of oversize is done by a hydraulic impact breaker mounted on a hydraulically operated articulated arm situated at the side of the dump pocket. Again because of the shallow pocket, no splitter is used to protect the spider of the 60 in. by 89 in. Traylor gyratory crusher, which is equipped with a hydroset mechanism. Crushed ore at 8 in. (203 mm) drops into the 360 st surge chamber lined with AR plate and then is fed directly to the 60 in. (1.52 m) stock- pile conveyor by an 84 in. by 20 ft (2. 13 m by 6.1 m) four-speed apron feeder at a rate of up to 4000 stph. Early in 1977, Cities Service will replace the four -speed electric drive with a hydraulic pump and motor with infinitely variable speed. They are also studying the replacement of the apron feeder with an 8 ft wide (2.44 m) belt feeder similar to those at Similkameen and Palabora. Peak crushing capacity would then be increased to 5000 stph. The AR plate in the crushed ore pocket was installed in large, rectangular sheets which required much less embedded metal to hold it in place than would the more conventional, smaller arid square pieces of cast manganese steel. For duty in the crushed ore pocket, where wear is not severe, the AR plate is a satisfactory material. The new Palabora Figure-8 crusher also uses this design.

Jan 1, 1978

By R. K. Matheson

THE Nivloc mine is 9 miles west of Silver Peak, Esmeralda County, Nevada. It has been operated by Desert Silver, Inc., since the summer of 1937. The cyanide mill treats 19o tons of silver-gold ore per day. In March of this year the main operations were about 2000 ft. west of the main shaft, which served as the downcast air passage for the mine. The mechanical blowers in use were sufficient to ventilate the west end at that time, but it was foreseen that as the mining area was extended ventilation would be an increasingly difficult problem, especially during the summer months. It was decided, therefore, to continue a raise from a point 100 ft. above the highest mining level (440-ft. level) to the surface; a distance of 443 ft. at approximately 65° From this point 40 ft. of drifting would be necessary to connect with a shallow shaft on the surface. (Fig. I.) All the raise was serviced from the 440-ft. level; costs and progress obtained in the initial 100 ft. are included in the following pages. CHOICE OF RAISE A raise in this locality would have four objects: (I) to provide an ample supply of fresh air to the working places; (2) to explore the vein from the highest mining level to the surface; (3) to provide waste fill for stopes in the area, and possibly provide a transfer for waste from the surface; (4) to provide an emergency exit in the west end of the mine. Before the mining of an ore shoot in the eastern part of the mine, a similar raise had been driven for purposes of ventilation and exploration. This raise and subsequent mining showed the vein to be noncommercial for a distance of about 250 ft. below the surface. However, in the area under operation, old surface workings showed occasional values. Thus from a development standpoint the raise was an excellent prospect. The raise chosen was a three-compartment, stulled raise having two chutes and a manway. The manway inside timber measured 4 ft. 8 in. by 4 ft. 6 in.; it carried air and water pipes, a ladderway and a slide for a timber skip. The two chutes would be used for drawing off the muck and the cleaning of the bulkhead, as well as for ore and waste passes, which would be especially useful for lateral exploration from the raise. The fairly large cross section of the raise (6 by 15 ft.) would provide a large quantity of waste for backfilling, and more could be obtained from a glory hole on the surface. TIME SCHEDULE As speed in completing the raise was the main requisite, three shifts were considered, but two shifts were decided upon when it was found that three would necessitate considerably larger fans than those available for clearing the raise. The main diffi-

Jan 1, 1942

By Ronald C. Koo

SMALL additions of potassium, aluminum, and silicon as oxides (referred to as dope) to tungsten have been known for several decades to have a very large effect in raising the recrystallization temperature and altering the recrystallized grain morphology of heavily drawn wire. Previous investigations of this doping effect1 6 have led to various speculations but all failed to deduce unequivocally the physical state or the mechanistic influence of the dopant. Recently, walter7 has observed, by transmission electron microscopy, strings of "fine particles" in heavily rolled and annealed doped tungsten sheet and concluded that they were particles of mullite (Al6Si2013). His conclusion was inferred from the electron diffraction patterns of large particles ex-trated by carbon replication of fractured surfaces of slabs rolled from sintered ingots. That the strings of "fine particles" in heavily rolled and annealed sheet were also mullite was an assumption for which no evidence was presented. A similar investigation has been carried out in this laboratory over the past 2 years on a variety of tungsten wire: doped tungsten, and undoped tungsten, as well as 218 doped tungsten purchased from the Lamp Metals and Components Department of the G.E. Lamp Division. Although the electron microscope observations are similar to those reported by Walter, the writer has reached a different conclusion concerning the physical state of the dopant in annealed tungsten. The purpose of this communication is to present evidence that the strings of "fine particles" observed in transmission specimens are not mullite, but are voids. In the present investigation, tungsten wire, 0.88 mm in diam, was rolled into ribbon 0.2 mm by 125 µ thick. The ribbons were annealed in vacuo at a pressure of -1 x 10-5 Torr and then thinned electrolytically in a 2 pct KOH solution. Fig. 1 shows a typical transmissicjn electron micrograph of a sample annealed at 1700°C for 30 min which reveals rows of closely spaced voids having a light contrast (referred to as "fine particles" by Walter) aligned parallel to the working direction. Stereo micrographs (by D. Moon, Westinghouse Research and Development Center) have shown that these voids do not exist on the surfaces of the specimens as a result of thinning but are within the thin-foil specimens. The following experiments have been performed to verify that these are indeed voids. I) Effect of Annealing. Voids are absent in unannealed specimens and appear only after annealing. This behavior cannot be explained if they were solid particles such as mullite. Precipitation (in an unquenched specimen) upon annealing requires solute elements having decreasing solubilities with increasing temperature. Although the solubility of aluminum in tungsten does decrease with increasing temperature, precipitation requires a concentration in excess of 1.4 wt pct,8 which is at least two orders of magnitude higher than the aluminum content in doped tungsten. It is also unreasonable to assume that particles aligned in rows initially present in unannealed specimens were too

Jan 1, 1968

By R. W. Raymond

to same extent, the assumptions tinderlying Dr. Ilu?ley's con alusions. These amrrmptions are: that 'the loss of metal per million tons of trafffc, depends, first upon the circrtnistances under which the rail is worn; secondly, upon the proportions of its various constituents, ancl that the anlorlnt of loss is afEect~d by eacb constitnent in a cer tain ratio, so that if the circunlstances were the same for all tlie mils, the wear per nliilion tons might he upproxi91ately expre~sed by an equation of the form I + Cc + Pp + SR + Mm = R, io wtlioh I is an unknown valne, dependi~.rg on the quantity of iron (and other ingre dients not determined) in the rail, and assumed to be constant for all the rails ; c, p, s, and m are the experimentally determined quan tities of carhon, phosphorus, sulphur, and manganese, as tabulater1 in YIates VT and VII of Dr. Dudley's paper; and R is the experirnen tdlly dcterlnincd wear per million tons; while C, P, S, and M are onknown wfficients. In other words, it is assunled that the differ ence in wear is proportional to a difference in c, p, s, or m, and that the effects of a change in the amonnt of either are independent of the amount of the rest-—within the experinlental limit5 of the problem. It is also assr~med that sulphar, copper, and other ingredients, not determined, are qually present in all the rails, or at least {lo not affect the wear, since I is taken as constant. Dr. Dudley tacitly assumes the coefficient6 C, P, S, and M to be positive; and assigns certain valries to them, by means of which he redom t.he equation to the form I + Pa: = R, x being equal to cc + Es +Mm i Pp, or tjje uanjbe,. of so-called phosphorus units in the rail. But we do not have R directly given under constant circumstances. The varying weights (per engine, car, or train) and the varying epds, we must neglect for lack of data, and assume that in these rwpects the rails examined have been treated srlbstantially alike. But there remain the varying conditions as to track, which mnst he elirninsted. Dr. Dudley gives six clrlsses, four of which contain 8 rails each, and two 16 rails each. Beginning with the 6~st (tangent grade), take the mean of the figures expressing wear for that clam; and continaing tliis process through the other five, we obtain six expressions in quantity of loss 'by wear, which we assome tc, represent, in their differences, the varying conditions of the trarli, with respect to grade and direction. We now take the mean of these moans (giving double weight to the gmiip containing 16 ohwrvafieras). This general rnean is the 10 of metal per million tons of trafio for a rail of avorage constitution under mean ciroumstances.

Jan 1, 1881

By G. H. Anderson

Cadmium-coppeR precipitate, a byproduct of the purification stage of the zinc plant, is composed mainly of zinc, cadmium and copper in varying amounts depending on the efficiency of precipitation and the cadmium and copper contents of the impure solution treated. The composition range is approximately: cadmium 10-12 pct, copper 6-8 pct, and zinc 3&35 pct. As received at the cadmium plant, the precipitate is a dark gray to black press cake produced by filter pressing the flocculent cadmium-copper precipitate formed when impure zinc solution is agitated with zinc dust. The details of the cadmium-copper precipitation are to be found in the paper "Electrolytic Zinc at Risdon, Tasmania," by W. C. Snow. Transactions AIME, 121, 501. The treatment, in addition to recovering cadmium as metal, yields a copper product as a residue for realization and recovers in solution for return to the zinc plant, the excess of zinc dust used during purification. The recovery of cadmium metal is approximately 200 tons† per year, but, with the amount of copper residue recovered, varies with the zinc production tonnage, composition of the original concentrates, degree of roasting and other operational factors. The operations involved in the recovery of the foregoing materials are carried out in a building adjacent to the purification section of the zinc plant and can best be described by dividing the process into the following stages: 1. Oxidation and Grinding of the cadmium-copper precipitate. 2. Leaching and Filtering. 3. Precipitation of cadmium. 4. Oxidation and Grinding of the precipitated cadmium. 5. Leaching oxidized cadmium precipitate and Purification of leach solution. 6. Electrolysis. 7. Melting, Casting and Packing. A feature of the process is the use of two distinct solution circuits. Spent electrolyte from the zinc plant circuit containing about 10 pct sulphuric acid is used as the primary solvent of the cadmium and zinc present in the oxidized precipitate. When the cadmium is later separated by precipitation and filtering, the filtrate, originally zinc plant spent electrolyte and now fortified in zinc, is returned to the zinc plant. The precipitated cadmium, after oxidation, is redissolved in spent electrolyte from cadmium electrolysis which solution is in closed circuit within the cadmium plant except for discards to the zinc plant circuit as mentioned in Section 5 hereinafter. (Fig 1.) Details of the various operations follow. I. Oxidation and Grinding of the Cadminm-copper Precipitate The precipitate having had a preliminary drying by compressed air in Dehne filter presses in the zinc plant is trucked to a storage platform of sufiicient length to store 3 to 4 days' production separately. After 48 hr exposure to atmosphere, oxidation is sufficient to enable all cadmium and zinc but only a portion of the copper to be dissolved in dilute sulphuric acid. The oxidized precipitate is shovelled into trucks and, after weighing and sampling, is broken in size by means of

Jan 1, 1950

By L. L. McMurray

ILMENITE is the most important raw material for manufacture of titanium dioxide.1 Industrially, several other products are made from ilmenite, the most important of which are: ferrotitanium, ferro carbon-titanium, copper-titanium, titanium carbide and titanium nitride. The production of titanium metal is still in the laboratory stage because of the difficulty of extraction and as yet no important application for the metal has been found. Ilmenite has received considerable attention as an industrial raw material. Imports of ilmenite concentrates for the first nine months of 1941 were 156,737 short tons, the chief source being Travancore, India.2 Domestic production of ilmenite has here-tofore been confined to Amherst and Nelson Counties, Virginia, where a complex rutile, ilmenite, and apatite ore is mined and treated to utilize all three of these minerals. A recent report3 has described development of the large titaniferous magnetite ore body at Tahawas, New York, where it is expected that 800 tons of ilmenite concentrates, containing 48 per cent Ti02 will be produced daily. Additional domestic production is expected from a large ilmenite deposit recently opened in Caldwell County, North Carolina. Flotation tests indicate that a high-grade concentrate containing 53 per cent Ti02 can be made from the North Carolina ore. Prospecting of domestic ores in other areas has been reported.4 It appears that increased domestic production of ilmenite may well save considerable shipping space so vitally needed in these times. The composition and chemical structure of pure ilmenite is given by Dana as: FeO, TiO2; Ti, 31.6 per cent, Fe, 36.8 per cent, 02, 31.6 per cent. This composition is variable in that some iron or titanium may be replaced, giving a variable iron-titanium ratio. As an example, the iron-titanium weight ratio of ilmenite in Caldwell County, North Carolina, has been determined to be 0.94 (using 97.1 per cent ilmenite concentrate obtained by heavy liquids on minus 150-mesh ore) compared with theoretical 1.16. No rutile was noted in this ore to account for the low value. This North Carolina ore is free of magnetite, which is a common associate of ilmenite ores. In view of a large potential production from North Carolina, the Tennessee Valley Authority conducted a study of methods of concentration of that ore, of which the results are reported herein. THE ORE Five samples of ore were taken from the deposit at various exposed locations and were mixed for the study and testing. An attempt was made to proportion the amount of weathered and unweathered portions in making the composite sample, so as to approximate actual operating conditions. An examination of representative specimens of the sample showed the following general facts: I. The black mineral comprising nearly 70 per cent of the ore is ilmenite.

Jan 1, 1944

SEC. 1. The membership of the Institute shall comprise six classes, namely: 1. Members; 2. Honorary Members; 3. Senior Members; 4. Associates; 5. Junior Members; 6, Rocky Mountain Members. All shall be equally entitled to the privileges of membership, excepting that no member of any class whose residence shall be outside of the United States of America, except those residing in Mexico and Canada, shall be entitled to vote. SEC. 2. Members: A person to be eligible for election or transfer into the class of Member must be at least 27 years of age and must have had at least six years' employment in the practice of engineering, mining, geology, metallurgy, or chemistry, during at least three years of which he must have held positions of responsibility in one or more of these fields. This shall not apply to Rocky Mountain members. SEC. 3. Honorary Members: Each candidate for Honorary Membership must be recommended by at least ten Members and must be elected by ballot at a meeting of the Board of Directors by the unanimous vote of the Directors present; provided, however, that the number of Honorary Members shall at no time exceed twenty. Such election shall automatically act as a transfer of such member from any other class of membership to which he may belong. SEC. 4. Senior Members: The Directors may in their discretion place on the Honor Roll of Senior Members and transfer from any other class of membership other than Honorary Membership the name of any Member or Associate who has reached the age of seventy years and who has paid dues for thirty years, and for good reasons in • special cases may vary the age or number of years. SEC. 5. Junior Members: A person to be eligible for election to the class of Junior Member must be qualified through education or experience to hold a subordinate position in engineering, mining, metallurgical, geological or chemical work. He shall be not more than twenty-seven years of age at the time of election. The rights of the present Junior Associates shall continue until the same expire by limitation of time. SEC. 6. Associates: A person eligible for election or transfer into the class of Associate shall be one, who, in the opinion of the Committee on Admissions and the Board of Directors, is suitable for such election or transfer by reason of his interest in or connection with mining, geology, metallurgy, or chemistry. SEC. 7. Rocky Mountain Members: Membership in a special class of life memberships without annual or other dues and without right to receive the printed literature distributed to other members or the right and privilege of wearing the official badge of technical members, is given to all members of the Rocky Mountain Club at the time of consolidation. These special Rocky Mountain memberships shall be claimable by any member of the Rocky Mountain Club, not already a member of the Institute,

Jan 1, 1929

By Emma Smith, R. W. Guard

INVESTIGATION of the nickel-rich end of the Ni-Zr system has been prompted by an interest in the effect of small amounts of zirconium in high temperature alloys. Hansenl presents a hypothetical diagram based on the work of Allibone and Sykes,2 who investigated the system up to 44 atomic pct (55 wt pct) Zr by metallographic means. Since the alloys they used were melted in Alundum crucibles they were probably contaminated with appreciable amounts of aluminum. They found two compounds which they called Ni3Zr and Ni4Zr. Hayes, Roberson, and Paasche3 identified a compound NiZr (50 atomic pct Zr) with a melting point of 1470°C. Such a high melting compound is not compatible with the observation of Allibone and Sykes2 hat a eutectic is formed near 50 atomic pct. The alloys containing up to 60 atomic pct Zr were melted in an inert atmosphere in a noncon-sumable electrode arc furnace. Analysis of most of the alloys indicated negligible loss of zirconium. The alloys were examined in the as-cast condition and also after annealing for 6 hr at 1175°C (or 1000°C for the alloys between 25 atomic pct and 45 atomic pct). Metallographic specimens were etched using mixtures of HF-HNO3-H2O or acetic acid- HN0,-H,O. The specimens for the solidus determinations were wrapped in molybdenum foil and sealed in evacuated quartz tubes. Specimens to be heated above 1300°C were enclosed in zirconia tubes inside the quartz to prevent reaction with molybdenum. The solidus determinations were carried out by heating the specimens at various temperatures for a few minutes and then examining the interior structure metallographically to determine at what temperature melting began. The 150 mesh powders for X-ray analysis were annealed in an evacuated quartz tube for 2 hr at 540 °C to remove cold work. Alloys with 22.5 atomic pct Zr and 44.4 atomic pct Zr required annealing at 700 °C for complete recovery. The grains of both of these alloys were soft and rather ductile. Both Debye-Scherrer film patterns and spectrometer traces were made for each alloy using filtered copper radiation. Results and Discussion The presence of a substantial amount of second phase in an alloy with 1.1 atomic pct Zr indicated that the solid solubility of zirconium in nickel is somewhat less than 1 atomic pct. The a0 value for the face-centered-cubic matrix in the same alloy was equal to that of pure nickel, so that the solubility must be very small. This observation is as expected from the large atom size difference. Annealed specimens of alloys with 15.0, 16.7, 22.5, 28.6, 44.4, and 59.4 atomic pct Zr showed. micro-structures that were essentially single phase. When

Jan 1, 1958