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By S. Frederick Ravitz

JUDGING from the inquiries that are constantly being received by the Utah Engineering Experiment Station as to the "Why," so to speak, of the flotation process of concentrating minerals, it occurred to me that perhaps a brief statement of the more important theories might interest those who have not followed the technical literature. Like many other industrial processes, flotation has hitherto been developed on an almost purely empirical basis, with relatively little practical contribution from the fundamental chemistry and physics on which the phenomena are based. In fact, its development by the trial - and - error method has been perfected to such a high state that it is becoming generally thought that further important advances can be brought about only by a thorough understanding of the actual mechanism of the process. Natur¬ally, such a complicated process has brought forth numerous theories, most of which have failed to withstand the test of time. It is significant that no theory has yet been advanced which is universally accepted.

Jan 1, 1933

By Walter White

THE measurement of the reading of a thermoelement is the measurement of an electromotive force extraordinarily small compared to those generally used in commercial work. Of the various possible methods of measuring such a quantity, the most advantageous is always a delicate galvanometer. Since a galvanometer measures current, it is necessary to adopt some scheme by which its current reading shall indicate electromotive force. There are two general methods of doing this. One is to use the delicate galvanometer as a "direct reader," that is, to let the electromotive force of the thermoelement furnish the power and produce the current measured. If the resistance is constant the reading will, after a suitable calibration, give the electromotive force of the thermoelement which, by means of a table or of a suitable scale in the galvanometer itself, will FIG. 1.-SIMPLIFIED POTENTIOMETER. POTENTIAL DROP ACROSS THE PART PIN or CIRCUIT OF BULL CELL BALANCES THAT OF THERMOELEMENT TC WHEN GALVANOMETER G READS ZERO. give the temperature. The other method, that of the potentiometer, is to balance the electromotive force of the thermoelement by means of another electromotive force, using the galvanometer to tell when the balance is made. The usual way of getting this other electromotive force is to have a battery, the "bull" cell, send a current through a series of resistances, which 'may in a special case be the resistance of a single wire. The fall of potential along this circuit will then, by Ohm's Law, be proportional to the resistance; the potential difference between any two points, proportional to the resistance between the two points. This is represented in Fig. 1, where M and N are the two points in the circuit AZ of the battery. If M or N, or both, is movable so that the resistance

Jan 9, 1919

By CHARLES F. DEISS

The total pipe-line runs of petroleum in Indiana during 1945 were 4,114,000 bbl., a decline of nearly 17 per cent below the estimated 4,950,000 bbl. produced in 1944. Drilling activity during the year was centered in Posey and Gibson Counties, where seven new pools were discovered in the state. Four of the pools are in Posey County-Crunk, Farmersville, Jeffries and St. Wendells East-and the other three are in Gibson County-Johnson West, Lysle and Mt. Carmel East.

Jan 1, 1946

By W. H. Ashby, R. W. Cassingham, C. R. Blomberg, J. B. Justins

The Brookhaven field is one of several Basal Tuscaloosa reservoirs located in south-central Mississippi. It is a standstone reservoir, of erratic deposition and with several faults, having an approximate subsea depth of 9,800 ft. A large variation in permeability exists with a weighted average being 256 md. Estimated average interstitial water saturation is 45 per cent. The undersaturated reservoir fluid exhibits marked differences in physical properties with measured saturation pressures ranging from 733 to 2,255 psi. Early rapid decline in reservoir pressure caused the operating interests to unitize the field and initiate a program of pressure maintenance by gas injection. At the time gas injection was commenced, the reservoir pressure had fallen to nearly half of the original pressure with only 4.5 Per cent of the original oil in place produced. The reservoir pressure has since been maintained at approximately 2,750 psig, and cumulative production to date is 17 per cent of original oil in place. An analysis of field performance during gas injection is presented in detail. The program of pressure maintenance by gas injection is considered to be a success, since the expected ultimate recovery has been increased and the current production rate is in excess of 2 per cent of original oil in place per year. Performance has been better, anticipated ultimate recovery is larger, and total production costs are lower than for a similar Basal Tuscaloosa reservoir nearby, even though that field appears to have a more effective natural water drive. INTRODUCTION The history of the Brookhaven Unit is a testimonial for unitization and for the application of engineering techniques in the operation of an oil field. The operating and royalty interests in this field have mutually benefited from their early recognition of the need for unitization and pressure maintenance and from the forthright manner in which these were accomplished. The tangible benefits accruing to the participants in the Unit are: (1) income from gasoline plant products, (2) reduced lifting and operating costs from those of competitive operation, (3) maintenance of high levels of current income by mitigation of the inevitable decline in production rates inherent to natural depletion, (4) an increase in ultimate recovery of about 40 per cent over natural depletion operations. This paper should properly be considered a progress report; however, the performance of the field after five years of pressure maintenance clearly indicates that the ultimate success of the project is assured. LOCATION AND GEOLOGY The Brookhaven field is located in south-central Mississippi, about six miles from the town of Brookhaven. Production at Brookhaven

Jan 1, 1955

By L. D. Mullins, H. B. Bradley

Numerous articles have appeared in the literature citing the application of the potentiometric analyzer to cycling operations. Specific information obtainable by a potentiometric analysis, as noted by various investigators, includes: 1. Pattern sweep efficiency for various injection and production rate programs. 2. Injected fluid breakthrough time at production wells. 3. Optimum production and injection rates. 4. Prediction of injection and/or production well locations. 5. History of advance of the in-jected-produced fluid interface. 6. Ultimate life of the reservoir. 7. Ultimate reservoir production. This note describes a procedure for predicting pressure distribution in a gas-condensate reservoir by using the potentiometric analyzer to obtain potential distribution data on an analog model of the reservoir and then applying Muskat's' equations. The method relates the volumetric weighted average datum pressure to the mean potential in the model.

Jan 1, 1958

By Fulton B. Flick

The micrography and macrography of aluminum and its alloys present certain difficulties. Many of the difficulties attendant on the micrography have been removed by methods developed during the past few years, notably those of E. H. Dix, Jr.1 The development of grain size in aluminum and its alloys may be equally troublesome, yet comparatively little detailed attention appears to have been given to it. Satisfactory reagents are available for the development of such structurcs in ferrous and most non-ferrous metals, but those applied to aluminum and its alloys, i. e., alcoholic or aqueous solutions of sodium hydroxide or hydrofluoric acid are not entirely satisfactory. Hanson and Arch-butt,2 in speaking of these two reagents, state that "These two reagents give fairly satisfactory results, but they sometimes produce badly tarnished surfaces from which the surface deposit is difficult to remove." It has been our experience that neither of these reagents is to be entirely relied on for developing structures suitable for study or photography. This means that when the etch fails to produce satisfactory results the specimen must be repolished, through the 000-paper at least, and then etched with another reagent. This procedure entails a considerable loss of time, and the final results may not be all that might be desired. However, the reagent to be described, although not a panacea for all etching troubles, has improved results so markedly that it is felt that it & worth offering as a grain-size etch generally applicable to aluminum and aluminum alloys. Czochralski3 in 1915 mentioned the application of a solution of 10 to 20 c. c. concentrated hydrofluoric acid in 100 c. c. absolute alcohol, etching in this reagent being followed by dipping in concentrated hydrochloric acid soliltion.

Jan 1, 1925

By John H. Smith, Michael B. Bever

Pure gold was deformed by wire drawing at room temperature and 78°K. After deformation at room temperature, the stored energy and the resistivity increment reached nearly constant levels at high strains, whereas the yield stress continued to increase with strain. After deformation at 78K, the stored energy, the reszstivity increment, and the yield stress were larger than after deformation at room temperature mzd increased continuously with strain. Annealing at THE stored energy and the changes in properties resulting from cold working of Au-Ag alloys by various processes have been the subject of a series of investigations in this laboratory.'-' The work reported here room temperature after deformation at 78°K did not affect the yield stress appreciably. The stored energy, resistivity increment, and Lncrease in yield stress after deformation at room te-lnperature can be explained primarily in lerrns of dislocations while point defects, as well as dislocations, contribute to the changes in these properties after deformalion at 78°K. extends this research to pure gold. The stored energy, the resistivity increment, and the tensile properties after deformation by wire drawing were measured as functions of the strain at room temperature and at 78°K. The effect of the testing temperature and the effect of intermediate annealing at room temperature before testing at 78°K on the tensile properties of gold deformed at 78°K were also investigated. wire drawing made it possible to use a large range of strains, which was desirable because previous work on the deformation of gold had been carried out mainly at relatively small strains.'-l2 Also, wire specimens

Jan 1, 1969

By Mark L. Requa

(San Francisco fleeting, October, 1911.) DURING the past two years California has developed a new and important oil-field : I refer to Midway. This field produced the famous Lake View gusher, which is credited with a total production in excess of 8,000,000 barrels. Fortunately for the oil industry of the State, this well is now a thing of the past, and nothing save a great crater-like opening marks its location. The pipe is entirely worn away and gone ; and it is a matter of serious doubt if there can be anything done that will cause the well to produce again. Fortunately, also, there have been no, other wells in that field or elsewhere throughout the State that in any way compared with the Lake View. Midway is noted for large wells, of from 500 to 2,000 barrels production; but the decline is rapid, and a few months serve to bring the output down to a few hundred barrels. In the oil-territory heretofore blocked out as proved and probable, there have been, during the year, many changes. Some areas which were expected to be fairly productive have apparently failed; others, more strictly "wild-cat," have come in; while in some of the older fields there are properties which are beginning to show evident signs of exhaustion. The total area of proved territory will therefore probably suffer but small increase, when balances are struck off. The increase of new area has come from extensions of the Midway field, the development of a field in Lost Hills and Belridge, and extensions of the Fullerton-Whittier field in southern California. In these later developments, down to date, the fresh area absolutely proved is not much in excess of 3,000 acres. Recent developments in Coalinga indicate the possible extension of that field to the south, but at great depth. Coalinga is still the most northerly field of any consequence in the State. The Kettleman Hills have hitherto brought in nothing, although a

Apr 1, 1912

[Abstmct of remarks by R. II. Sweetser arid suhscqueut discussion at the New York Meeting, February, 1926. The Transactions mill ultimately contain a report of work resulting from these discussions. Need for a standard of ualuration.—There should be an accepted method for evaluating the different kinds of bituminous coals based on their carbon just as that for iron ores is based on iron. Variation in the classes of coals and their desirability fol the different industrial uses is analagous to the case of iron ores. The iron people have developed a standard. In the past coals have not been intelligently distributed because the public has not been informed as to its uses. Many operators have known nothing about the final disposal of the coal shipped from their mines. Sales agents and retailers have had no means of evaluating coals except to make the price as high as the market will stand. Producers and distributors need to know how much more valuable the coals would be if prepared so as to contain less objectionable material. Mr. Swectser cnlletl on the Goal and Coke Committee of the Institnte to organize a study through producers and users to develop a method scientifically and comnereially sound E. A holbrook said that the information exists but the public is unwilling to investigate. He praised Ashley's1 nomenclature of the different kind of coal which has been accepted by the Coal Mining Institute of America and recommended to the American Enginecring Standards Commitee. G. S. Rice pointed out the wider variety and distribution of consumption of coal compared to Iron ore. C'. M. Young approved Mr. Sweetser's remarks and hoped lor a research institution, probably endowed, to study utilization of coal after it comes from the ground. Mr. Sweetser cited incidents to prove his former statements. He said that a reduction of 1 per cent. ash in the coal would cut down the cost of pig iron at a blast furnace 30 c. a ton, that the coal men should tell what the iron men would have to pay to get better coal. H. J. Prryn endorsed the need of blast-furnace operators to know the kind of coal from which their- coke is made and the latler's ash content, as this affects coke consumption. A. C. Fieldncr explained that the difficulty of evaluating coal on the basis of chermical analyses for calorimetric tests is: (1) representativr

Jan 1, 1927

By Charles Will Wright

THE HIGHLY SPECIALIZED heavy air transport services to mining regions, such as exist in the New Guinea gold fields and in northern Canada, have been even more essential in the development of mines in Peru. Few nations have been con- fronted with greater natural obstacles to transport than has Peru, and without the plane it would have been impossible to get the machinery and supplies for the construction of power plants and mills to many of these interior mines, situated as they are over high mountain ranges, with muleback the principal means of transportation. As the mines within a district become important producers and warrant the expenditure, the mule trail is being replaced by automobile roads to connect with the railway stations and with the airports.

Jan 1, 1940

NEW MEMBERS The following list comprises the names of those persons who became members during the period of Apr. 10, 1917, to May 10, 1917. ANDERSON, GEORGE K., JR., Supt., Iron Ore Mines, The Low Moor Iron Co. of Va., Longdale, Va. AVERY, DAVID, Met Collins House, Collins St., Melbourne, Vic., Australia. BATES WILLIAM T., Shift Foreman, American Zinc Co. of Tenn., Mascot, Tenn. BIRD, ELMER, Min. & Civil Engr P. O. Box 1483, Boise, Idaho. BLACKBURN, JOSEPH R., Vice-Pres. & Genl. Mgr., Austen Coal & Coke Co., Austen, Preston Co., W. Va. BOTSFORD, FRANK P., Asst. Genl. Supt., Eastern Mesaba, Pickands Mather & Co., Gilbert, St. Luis Co., Minn. BRADEN, SPRUILLE, Min. Engr., Andes Exploration Co. of Maine, Casilla 83-D, Santiago, Chile South America. BROWNE, DAVID G., Mill Designer, New Jersey Zinc Co., 55 Wall St., New York, N. Y. BRUDERLIN, EMIL J., Met. Engr., Ohio & Colorado Smelt. & Ref. Co., Salida, Colo. CAMPBELL, DONALD C., Min. Engr., Campbell Wells & Elmendorf, 114 James St., Seattle, Wash. CARRIGAN, J. J., Asst. Genl. Supt. of Mines, Anaconda Copper Min. Co., Butte, Mont.

Jan 6, 1917

By G. K. Burgess

G. K. BURGESS* and R. W. WOODWARD,? Washington, D. C.-From a metallurgical standpoint, there are several ways in which a reduction of the tin consumed in commercial non-ferrous and white-metal alloys can be effected. First, a reduction of the tin, content of the alloy; second, substitution of part or all of the tin content by some other metal; third, a substitution of a different type of alloy, which in some cases also involves a change in mechanical design. The Bureau of Standards has been studying these methods of conservation for tin alloys, particularly in regard to babbitts and bearing metals, bronzes, and solders. Much of the information secured by the Bureau was obtained from answers to questionnaires sent to manufacturers and users of these materials, so that, in general, any of the following suggestions or recommendations can be considered as being practical and as having already been thoroughly tried. Bearing Metals There is no question that the tin content of nearly all bearing metals can be reduced to some extent, and in some cases actually eliminated

Jan 12, 1918

Papers published by the Institute are issued in a variety of forms MINING TECHNOLOGY, issued every other month, contains the TECHNICAL PUBLICATIONS on Metal Mining, Minerals Beneficiation (milling and concentration), Industrial Minerals (nonmetallic) and Mining Geology, Mining Administration, and Geophysics papers relating to Metal Mining (A, B, H, I, K, L ) METALS TECHNOLOGY, issued eight times a year, contains the TECHNICAL PUBLICATIONS of the Iron and Steel Division and the Institute of Metals Division, and once or twice during the year those on Non-ferrous Metallurgy (reduction and refining of nonferrous metals) (C, E, and D ) PETROLEUM TECHNOLOGY, issued every other month, contains the TECHNICAL PUBLICATIONS of the Petroleum Division, together with Geophysics papers relating to -the finding of Petroleum (G, L ) COAL TECHNOLOGY, issued four times a year, contains the TECHNICAL PUBLICATIONS of the Coal Division (F ) MINERAL INDUSTRY EDUCATION DIVISION papers appear in a TECHNOLOGY according to classification of subject matter DISCUSSIONS appear in the respective TECHNOLOGY as available MINING AND METALLURGY is the monthly magazine, which contains papers of general interest and news of the membership

Jan 1, 1952

By H. W. Highriter

THE method developed and used in this laboratory for the production of metallic uranium of such purity that it is ductile and can be cold-worked to fine wire or thin sheet by rolling has already been described1. It consists, briefly, in the electrolysis of potassium uranous fluoride (KUF5) in a molten bath composed of equal parts of sodium and calcium chlorides. The bath is contained in a graphite crucible, electrically heated to about 775° C., the crucible serving as the anode for electrolysis. The uranium deposits in finely divided form mixed with salts upon a molybdenum cathode suspended axially in the crucible. Upon com-pletion of the electrolysis the cathode is removed and cooled, the deposit broken and leached to remove salts. The metal powder is washed with water and dilute acetic acid and dried in vacuo to reduce oxidation. Suitable amounts are then pressed into pellets and heated in vacuo by high-frequency induction, using a thoria crucible. The uranium melts and flows away from the pellet, leaving a shell, which is largely oxide. In general, this method produced a satisfactory metal, although at times the uranium was not ductile. The investigations recorded here were made to find the cause of this embrittlement. It was known that the metal generally contained carbon, derived from disintegration of the graphite crucible in which electrolysis is conducted, in amounts dependent upon the thoroughness of washing the metal powder. Accordingly, analyses of several samples, both ductile and brittle, were made by combustion and absorption of C02 in Ascarite, using air instead of oxygen to reduce the temperature and rate of oxida-tion. Several of these metals were made with special precautions to reduce carbon content. The results show no relationship between ductility and carbon content in the range investigated (Table 1).

Jan 1, 1935

By Benjamin Gi ldersleeve

Uniquely colored, thin-bedded quartzite is quarried between Crossville and Crab Orchard in Cumberland County, Tenn. It is produced in all sizes up to the limits of transportation from beds usually ranging in thickness from less than 1/2 in. to 6 in. The stone is very resistant to wear and weathering and is marketed throughout the country for many different purposes in exterior and interior construction. The annual production exceeds 36,000 tons, valued at nearly $1,000,000.

Jan 1, 1950

By W. A. Backofen, D. H. Avery, G. A. Miller

An evaluation has been made of the relative importance of yield strength (?) and stacking-fault energy (y) to the rate of fatigue-crack growth in materials of fcc structure. Pure copper and its solid-solution al-loys with aluminum and nickel were chosen for the study because they provided sufficient range in both quantities of interest that either could be varied independently of the other. Experiments involved alternating tension and compression of flat specimens which were prepared with sharpened internal notches so that most, if not all, of the crack-nucleation interval could be eliminated. Growth rate (dC/dN) was concluded to be proportional to the square of the plastic-strain amplitude (€,,) over a strain range of approximately 6x 10-4 to 6 x 10-3. The factor, k, linking dC/dN and ep in dC/dN = kEp2 increased and decreased with corresponding variations in y, but it did not respond syste?>/atically to change in ay, indicating that y is the significant variable in crack growth at constant plastic-strain amplitude. In polycrystalline material, k varied by a factor of 5 over the available range of y. In a few single-crystal experiments on Cu-A1 alloys the growth rate responded less strongly to change in y. It has been suggested that single crystals behave somewhat differently than poly crystalline material because there is more extetnsive substructure near the grain boundaries in the latter, and this facilitates crack advance by separation along subgrain boundaries. A point of some controversy in current work on fatigue relates to the effects of strength and stacking-fault energy on crack growth. In recent experiments a separation was made between the cycling intervals for crack nucleation and the subsequent growth that eventually ends a specimen's fatigue life.' The study was carried out on Cu-A1 alloys primarily, fatigued in alternating four-point bending to constant deflection. A nucleation interval of about 10' cycles (at a total strain amplitude = 0.2 pct) was found to be insensitive to aluminum content in the range 0 to 7.5 wt pct, while the growth period was increased approximately forty fold over the same compositional range. The increase was not in any sense linear, however. Rather, most of the change occurred below 4 pct A1 or a stacking-fault energy, ?, of about 15 ergs per sq cm. It was argued that the plastic-strain amplitude was approximately constant, and therefore the effect of composition must have grown out of the reduction in stacking-fault energy. Several studies have shown that, with high ?, cross slip is encouraged, subgrain structure is introduced during fatigue, and cracking is aided through propagation along subgrain boundaries.1-5 Therefore, lowering ? sufficiently to interfere with substructure formation would be expected to retard growth rate. On the other hand, it is a general rule that resistance to fatigue cracking increases as strength is raised. Accordingly, there might still have been some doubt that Y was the controlling variable, since strength would be increased as y was lowered by the aluminum additions. To help in dispelling that doubt, an experiment was made on a polycrystalline Cu-Ni alloy similar in strength to the Cu-A1 alloys but of higher ?; the crack-growth interval was found to be essentially that of pure copper.' Further support for this position on stacking-fault energy as it relates to crack growth is derived from work by Boettner and McEvily,6 in which the actual crack-growth rate was measured on samples previously notched so as to minimize the nucleation period. Unfortunately, it was necessary in isolating strength level to compare different alloy systems and grain sizes. Recognizing the complication, it was still concluded that growth may be retarded by a reduction in y, per se. A related study has also been made by Roberson and Grosskreutz.7 The zinc content of a brass was systematically changed to alter strength and stack-ing-fault energy, although not below the 15 ergs per sq cm at which pronounced change in growth interval was found in the earlier work. The results were limited to more or less conventional S-N diagrams so that nucleation and growth events could not be separated. No definite conclusions were drawn, but

Jan 1, 1967

The General Committee met in the Treasury Building at Washington on Oct. 6 and 7. At the first meeting, Cornelius P. Kelley was appointed chairman, and Paul Armitage, secretary. Sub-committees were ap-pointed on Invested Capital, Mine Valuation, and Depletion and De-preciation. On Oct. 7, the reports of these committees were submitted to the General Committee and were referred to the Executive Committee. A motion was carried that the Executive Committee he constituted a permanent committee to continue the work of the Committee, with full power to acid to and increase its membership, that. as thus increased, it should constitute a permanent organization to act- and cooperate with the Treasury Department in matters of mining taxation under the Federal Income and Excess Profits Tax Laws. Thereafter the Executive Com-mittee met and formed a permanent committee as follows: Cornelius F. Kelley, chairman, 42 Broadway, New York City. J. L. Darnell, office of the Commissioner of Internal Revenue, Wash-ington, D. C. J. Parke Channing, 61 Broadway, New York City. Walter Douglas, 99 John St., New York City. R. V. Norris, 542 Second National Bank Bldg., Wilkes-Barre, Pa. J. E. Spurr, Engineering and Mining Journal, 10th Ave., and 36th St., New York City. W. G. Swart, 808 Selwood Bldg., Duluth, Minn. J. P. Finley, 45 Cedar St., New York City. W. A. Williams, Bartlesville, Okla. F. S. Peabody, Peabody Coal Co., McCormick Bldg., Chicago, Ill. Matthew C. Fleming, 71 Broadway, New York City. H. B. Fernald, 54 Wall St., New York City. William G. Mather, Cleveland, Ohio. Walter Fitch, Eureka, Utah. Arthur Thacher, 900 Security Bldg., St. Louis, Mo. John P. Gray, Coeur d'Alene, Idaho. Paul Armitage, secretary, 233 Broadway, New York City.

Jan 12, 1919

One Hundred Sixteenth Meeting of the Institute, Monday, Feb. 18, to Thursday, Feb. 21, inclusive, 1918 A preliminary program, for the New York Meeting was printed in the January Bulletin, and a more detailed program was mailed to all members early in January. The following schedule is the outcome, of sundry committee meetings up to the middle of January. Committee on Arrangements J.` E. JOHNSON, JR., Chairman BRADLEY STOUGHTON, Vice-Chairman RALPH W. DEACON MRS. S. J. JENNINGS E. M. SHIPP J. V. N. DOER A. R. LEDOUX G. D. VAN ARSDALE L. `V. FRANCIS . . F. T. RUBIDGE ARTHUR L. WALKER Summarized Program MONDAY, FEBRUARY 18 9 a. m. to 5. p. m. Registration at Institute Headquarters. 10 a. m. Sessions on Coal and Non-Ferrous Metallurgy. 12.30 p. m. Luncheon at Engineering Societies'. Building. 2 p. m. Visit to Subway Workings.

Jan 2, 1918

By G. Das, S. V. Radcliffe

The substructural features developed in tungsten as a function of annealing temperature (up to 2200°C) and type of material [undoped and doped powder metallurgy (PM) tungsten and electron beam melted tungsten] have been investigated by transmission electron microscopy. For doped PM tungsten wires, characteristic "par-ticulate" substructural features developed rapidly with increase in annealing temperature above 700°C. The features consisted of parallel rows of elongated or circular shapes (500 to 1000A diam) lying along the direction of the wire axis and were identified as internal voids by diffraction contrast experiments. In recrystallized doped PM rod, larger voids were observed and were identified by precision dark field analysis to be cubic in shape and bounded by (100) planes. In marked contrast with both the doped PM materials, recrystallized undoped PM rod exhibited only very occasional and randomly arranged voids. Furthermore, no voids were observed in either material after electron beam melting. The high concentration of voids in the doped PM materials is attributed primarily to vaporization of doping additions or their pvoducts situated at the original grain boundaries , whereas the few voids in undoped material are considered to be traces of microporosity which were not eliminated during sintering. A tentative mechanism is suggested for the dezlelopment of the voids in relation to the processing sequences (sintering and working) and to the subsequent annealing. In recent years, a characteristic substructural feature consisting of rows of small elongated or circular regions of light contrast lying along the direction of working has been seen in thin foil electron microscopy studies of annealed sheet, wire, and rod tungsten. These features were present in the published micrographs of sheet by Weissmann et al.1 and of wire by Meieran and Thomas2, although the authors did not draw attention to them. Wronski and Fourdeux3 observed similar features in sintered rod tungsten (it was not specified whether or not the material was doped*) and interpreted them on the basis of their ap- particles, based on extraction replica evidence from the fracture surface of the initial hot-rolled slab material from which the sheet was prepared. No diffraction contrast experiments on the features were reported in any of these studies. The present investigation was undertaken with the primary objectives of: a) identifying the nature of these substructural features in tungsten by electron diffraction contrast experiments, since the contrast for voids can be expected to differ from that for crystalline or glassy particles, and b) elucidating the origin of the features and their development. For the latter purpose, doped and undoped powder metallurgy tungsten was obtained as rod and wire to represent different stages of reduction during final processing. These materials were examined both in the as-processed condition and after annealing to successively higher temperatures. In addition, the same doped and undoped materials were examined after vacuum melting in rod form. I) MATERIALS AND PROCEDURE Doped powder metallurgy (PM) tungsten wire (commercial purity 99.9 pct W) was obtained in the as-drawn and surface ground condition (0.030 in. diam "ground seal rod"). Doped and undoped tungsten rod (0.075 in. diam) representing an earlier stage of final processing was obtained from the same commercial source (Refractory Metals Division, General Electric Co.). Lengths of both the doped and undoped rod materials were single-pass melted in an electron-beam zone refiner to examine the effect of vacuum melting on the substructure. Annealing was carried out in a tungsten crucible in a tantalum strip resistance furnace under a vacuum of l0-15 mm Hg. Longitudinal sections of the wire and rod materials were examined by light and electron microscopy. The preparation of thin foils suitable for electron transmission from 0.030 in. diam tungsten wire and the rod specimens was carried out by means of a high-precision microjet technique developed to provide lack of jet stability and precise control of the area thinned. The method is described in detail elsewhere.' The foils were examined in a JEM 6A electron microscope using a goniometer stage (±20 deg tilt, 360 deg rotation) and operated at 100 kV. To minimize contamination problems a 200 µ condenser aperture was used in conjunction with a useful beam current of 50 µA. II) RESULTS AND DISCUSSION A) Diffraction Contrast Analysis. In order to determine the optimum conditions for the development of the substructural feature, a series of isochronal 30 min annealing experiments were carried out on specimens of the doped PM tungsten wire. The transmission electron microscopy analysis showed that the as-drawn wire, Fig. 1(a), consists of 'fibers' whose long axis is closely parallel to the wire axis of (110). The fiber width averages some 0.5 µ. Dense disloca-

Jan 1, 1969

By M. E. Learmont, R. J. Lipp, I. Iwasaki

In the selective flocculation of iron ores, the concentration of alkaline earth ions in pulp solutions plays a critical role. Sodium silicate, alone or with sodium tripolyphosphate, has been used as a dispersant. When Ca+ + concentration exceeds 15 to 20 ppm, however, only a strong complexing agent, such as ethylenediaminetetraacetate (EDTA) was found to be effective (Heerema, Lipp, and Iwasaki, 1979). Some iron ores release Ca+ + in excess of 20 ppm. With ores that contain gypsum, the Ca+ + concentration may reach several hundred ppm. The purpose of this investigation was to compare the effectiveness of EDTA with nitrilotriacetate (NTA) in countering the adverse effects of Ca+ +, particularly at high Ca+ + concentrations. Emphasis was placed on the use of NTA since it is more cost-effective than EDTA. It is also used in detergents in some countries (Malaiyandi, Williams, and O'Grady, 1979). NTA, like EDTA, forms a soluble complex with Ca+ + with a 1:1 molar ratio. Its structure and the value of log Kca are given below together with EDTA (Shibata, 1963). [ ] For experimental materials, an equal weight mixture of Lac Jeannine hematite and a high-purity quartzite from Thompson, MN, both ground to - 30 µm (- 560 mesh) was used. Selective flocculation test conditions and procedures were identical to those used in previous investigations (Heerema, Lipp, and Iwasaki, 1979). The optimum level of starch addition for the above mixture was determined to be at 300 g/t (0.6 lb per st). Initially, a series of selective flocculation tests were performed on the mixture pulped with 10-3M CaC12 (40 ppm Ca + +) at pH 11. With no NTA present, flocculation of the entire suspension resulted. The selectivities achieved in tests with 90, 100, and 150% of the stoichiometric amount of NTA were virtually identical to each other and also to the selectivity of separation obtained in the absence of Ca+ + Such an observation could have been expected since Ca+ + concentrations up to a few ppm may be tolerated in selective flocculation (Krishnan and Iwasaki, 1982). A similar series of tests were performed at 10-2M CaC12 (400 ppm Ca+ +). The results are shown in Fig. 1 as grade¬recovery curves. For comparison, the results obtained in the absence of Ca++ are included. At 90% of the stoichiometric amount of NTA, a large enough concentration of uncomplexed Ca+ + was left in solution to cause indiscriminate flocculation. Note in this figure that NTA is capable of countering the adverse effect of Ca+ + even at this high concentration when it is used in excess of stoichiometric amounts. The free Ca+ + concentrations at 100 and 150% are calculated to be 2.5 and 0 ppm, respectively. [ ] The relative effectiveness of NTA and EDTA was then compared at 100% of the stoichiometric amount using 10-2M and 10-3M CaCI2 (Fig. 2). EDTA appears to be slightly more effective than NTA. The free Ca++ of 0.02 ppm in 10-2M CaC12 with EDTA compared to 2.5 ppm free Ca+ + with NTA might account for the difference. As evident, prohibitively high additions of EDTA and NTA were required to complex high concentrations of calcium ion. The use of both of these agents would result in the accumulation of complexed Ca+ + in recycle water.

Jan 1, 1985