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By Donald B. Hunter

The Ti-Be system up lo 10 wt pct Be with cortlmercialll' pure titanium has been determined using metal-lographic techniques. Beryllium forms the p eutec-toid type of dinqarz with titanium; the eutectoid occurs at 0.5 xt pct Be azd 1500 F, while an eutectic is foritled at 1887°F containing between 5 and 7.5 rt pct Be. The solubility of beryllium in a titanium does not exceed 0.05 zvt pct and the maximum solubility of Beryllim in 0 titanium is 1 wt pet. PREVIOUS work on the Ti-Be phase diagram indicated that additions of beryllium to titanium resulted in a marked lowering of the melting point,''' and it was also observed that the solubility of beryllium in both a and p titanium was retricted.- With the limited data available, McQuillan and McQuillan constructed a partial hypothetical diagram of the Ti-Be system,= assuming that beryllium formed the 0 eutectoid type of system with titanium. Subsequently Bedford published a tentative diagram of the entire Ti-Be system: although he did not investigate alloys containing less than 10 wt pct Be. This diagram included several compounds described by other authorities.'-l3 The following account describes work directed toward determining the form of the titanium-rich portion of the phase diagram up to 10 wt pct Be. MATERIALS AND METHODS Titanium sponge and a master alloy containing 25 wt pct Be were used in the formulation of the alloys; the chemistry of these materials is detailed in Table I. The alloys were prepared as 250-g compacts which were melted into buttons by arc melting under purified argon on a water-cooled copper hearth. Results of analyses for beryllium are shown in Table I but no determination of other elements was made at this stage. The alloys were hot-rolled at 1650°F to produce 0.1-in.-thick sheet. Alloys containing up to 1.5 pct Be were fabricated without trouble; samples containing 2 pct cracked initially upon hot rolling, but thereafter rolled satisfactorily to sheet. The 5, 7.5, and 10 pct were hot short and could not be rolled. Surface contamination was removed from samples by sandblasting and pickling in a 5 pct HF-35 pct HNOs solution. For metal log raphic examination, heat-treated specimens were mounted transverse to the rolling direction, ground on silicon carbide papers of increasing fineness to 600 grit, and electropolished at 20 v using a solution containing 600 ml of methanol, 60 ml of perchloric acid, 360 ml of butyl cellosolve, and 2 ml of Solvent "X". Difficulty was experienced in obtaining good electropolished surfaces with samples containing more than 1 pct Be, the degree of difficulty in-

Jan 1, 1967

Page McGREGOR, A. G.-Features of the New Copper Smelting Plants in Arizona. Discussed by L. D. Ricketts, E. P. Mathewson 2145 HOWARD, L. O.-The Basic-Lined Converter in the Southwest. Discussed by Walter Douglas, E. P. Mathewson, Kuno Doerr 2145 SAMUEL, J. MOORE-Determination of Dust Losses at the Copper Queen Reduction Works. Discussed by Walter Douglas, E. P. Mathewson, S. J. Jennings, C. E. Arnold, A. G. McGregor, L. D. Ricketts 2148 MORSE, H. W., AND TOBELMANN, H. A.-Leaching Tests at New Cornelia. Discussed by H. W. Morse, Lawrence Addicks, G. D. Van Arsdale, S. J. Jennings, F. S. Schimerka, C. G. Grabill, F. N. Flynn, Stuart Croasdale 2151 LAIST, FREDERICK, AND ALDRICH, HAROLD W.-The 2,000-Ton Leaching Plant at Anaconda. Discussed by F. N. Flynn, E. P. Mathewson 2159 ADDICKS, LAWRENCE-Possibilities in the Wet. Treatment of Copper Concentrates. Discussed by F. N. Flynn 2160

Jan 12, 1916

By Gregory M. Dexter

Recent litigation in Pennsylvania between three coal-mining companies and a private water company resulted in the payment by the coal companies of the equivalent of about $500,000 to buy a new water supply to replace that which had been damaged by acid drainage from strip mining. An investigation of the relevant facts indicates that the water could have been treated by spending about $40,000 on equipment and $15,000 yearly for chemicals, labor, and power until the contarnination could be reduced about 80 pct. The water company's supply, furthermore, had deteriorated largely by reason of dry weather before stripping was begun by the coal companies. Payment to the water company should not have exceeded $300,000 and could have been as low as $100,000. Strip mining of coal is common in Pennsylvania. The most important objection to it in Pennsylvania is generally acid pollution of runoff water. An outline of the methods, therefore, that could be used to reduce such pollution, to compare acid-contaminated waters. and to treat such waters to make them satisfactory for public and industrial use is worth-while. The watershed of the West Penn Water Co. covers about 4.5 square miles, 20 miles west of Pittsburgh, and has two 90,000,000 gal reservoirs supplying about 1,300,000 gal daily for public and industrial use of which 450,000 gal daily are for two railroads. The pollution arises from weathered derivatives of typical'" Coal Measures"' rocks, the principal source being pyrite (and marcasite) in Pittsburgh and Rooster coals. Springs and seeps on hillsides issue from sandstone and limestone formations intersecting shale or clay land surfaces, or from perched water tables. The two reservoirs create an artificial permanent water table. Soap-hardness tests on three seepage samples taken in a dry summer ranged from 150 to 500 ppm. Water sampled came from aquifers above Pittsburgh and Rooster coals, obviating the possibility of contact with pyrite-containing coal. Since acid contamination of mine waters is the result of chemical reactions of oxygen and water with pyrite, it will be reduced by the exclusion of either air or water. The Sunnyhill Coal Co. has applied this principle in its "contouring" method of strip mining by burying contaminated coal-waste material under a compact, smoothed-up surface of top-soil, gravel, clay, and sand at a cost

Jan 1, 1950

The following discussion was held on August 2.2, 1927, during the meeting of the Institute at Salt Lake City. It. IIIatch, Garfield, Utah.—The object of the meeting, I belicve, is to determine the proper chemical composition to insure long wear of a ball in a mill. This might also apply to rods. I feel that there is only one way of determining accurately the wearing qualitites of balls in mills, and that is by actually wearing out 400 or 500 tolls of different kinds of balls. Two things add to the wearing qualities of a ball: (1) the tenacity, with which the particular particles of iron or steel are cemented together; (2) the individual hardness of each partiele. My cxperience is that a ball that has a Brincll of 550 to 650 will give comparatively long life. There is considerable difference of opinion as to the best steel and iron alloys neressary to produce a satisfactory grinding ball. Some favor chrome, somr manganese and some nickel. Personally, I believe cast iron alloyed with chrome makes the best ball for small sizes; for large sizes (31/2 in. arid up) steel alloyed with mangancse is best. L. O. Howard, Pullman, Wash.—How would this method apply to hning? A. Kissock, New York, N. Y.—I do not subcrribe to that exactly. As I am connected with the Climax Molybdenum Co. you would hardly expeet me to. We have been much interested in trying to work out this grinding-ball problem and have spent a, great deal of thought and effort on it. As we are associated with the American Metal Co. and have a number of Proprrties of our own, we are in poaition to try our ideas on ourselves first. We have tried different compositions, but, have not done anything very remarkable with them yet,, except that we have been able to say that the combination of chrome and molybdenum has given the best, wearing ball. Mr. Hatch feels that iron is the best. medium for grinding, hut since toughtiess as well as hardness is a factor in wearability we feel that a well made steel is better for this purpose. Another difficulty with cast, or chilled, iron is lack of uniformity front day to day or from heat to heat, and the impossibility of protlucing balls free from blow or shrinkage holes which matcrially affect their life. If cast iron is made hard it becomes brittle and lacks strctc11 or toughness. This prevents its use in the larger sizes, aS break:lgc, is a sorious hantlic:~p to efficiency. We have trirtl hard and brittle balls and softer but very tough balls and have proved that maximum hardness, with sufficient toughuess to prevent hrcakagv, is the most important factor. in resistarnce of a steel to abrasion. It is well known that. chromium is one of the best hardening agencies for cither iron or. steel; and molybdenum is recognized as an clerment capable of introducing tonghness. In other words, the proper combination of chromium and molybdenum permits unusual hadness with still sufficient touglmess to stand up under severest impact. It is yet too early to give any actual mill results of this new Combination and though we are proving our ideas at our own properties we have to depend on others to help us make the data more general and more worth while and would like to get some testa 206

Jan 1, 1928

By Albert Sauveur

IT is not without some hesitation, and even misgiving, that I venture into a discussion of the now classical Roberts-Austen Roozeboom diagram, lest I too fail, like so many other writers, in giving a satisfactory and logical explanation of these interesting curves. Roozeboom's original diagram is reproduced in Fig. 1. The generally accepted meaning of the various curves has been so often described before this Institute that it will suffice to recall it briefly before passing to my own interpretation of the changes involved.

Nov 1, 1906

By AIME

Lewis E. Young, who will formally assume his duties as President of the AIME at the Annual Meeting in San Francisco in February 1949, was born in Topeka, Kansas, Oct. 1, 1878. Dr. Young received his engineering education at the Pennsylvania State College, where he received the degree of B.S. in Mining Engineering in 1900. In 1904 he received his E.M. degree from Iowa State College, and in 1915 a Ph.D. from the University of Illinois. In 1947, the University of Missouri conferred on Dr. Young honoris causa the degree of Doctor of Engineering. His active career began in the educational field as instructor at Iowa State College, and following that, as professor of mining at the Colorado School of Mines, 1903-1907. While he was at Golden he launched hi: career as consulting mining engineer for various Western companies. Leaving the Colorado School of Mines, Dr. Young returned to Missouri, serving the University of Missouri as director of the School of Mines and Metallurgy at Rolla, 1907-1914. Leaving Missouri he went to the University of Illinois as assistant professor of business organization, 1915-1918, during which period he wrote exhaustive treatises on mine subsidence and mine taxation, which won for him the degree of Ph.D. before mentioned.

Jan 1, 1949

By Daniel R. Shawe

Large tabular beryllium deposits in waterlaid rhyolitic tuff at Spor Mountain, Utah, contain the world's largest known resources of beryllium (as bertrandite). The district also has produced fluorspar and uranium. The largest beryllium deposit is about 2.5 miles long, and known deposits contain many million tons of material with at least 0.5 per cent BeO. The beryllium-bearing tuff (Pliocene?) underlies topaz-bearing rhyolite ( Pliocene?) that contains unusually high amounts of beryllium, fluorine, and uranium, and overlies other volcanic rocks (Pliocene? or Micocene?) and marine carbonate and elastic rocks ( Paleozoic). The deposits occur in hydrothermally altered tuff only where it contains abundant carbonate pebbles eroded from the Paleozoic rocks and where the tuff was deposited as thick layers in now-buried paleovalleys. Basin and Range faults, thrust fa ults, and possibly strike-slip faults formed in this part of the Basin and Range province during the late Tertiary, and volcanic rocks were extruded. Beryllium mineralization probably occurred during this episode. Undoubtedly the beryllium deposits are related genetically to the topaz-bearing rhyolite, but the details of their genesis are not certain and probably are complex. Beryllium deposits are close to major faults, and locally the beryllium is concentrated at faults, indicating fault control of mineralization. Some elements in the deposits, such as lithium, however, are evenly distributed in certain Luff beds and perhaps were introduced prior to faulting. Still other elements, such as manganese and lead, were concentrated in the beryllium deposits and subsequently were leached along late fractures, indicating a period of metal redistribution following mineralization.

Jan 1, 1968

By AIME AIME

TWO weeks ago the writer was lunching in the Engineers` Club in New York with a man who has perhaps the widest acquaintance among engineers of anyone in the country a member of another of the Founder engineering societies. "By the way," lie asked. "who have they nominated for your next president."' "Doctor Becket," I told him- "Oh. that's line," he replied, in a heartfelt tone that rang with sincerity. "I have come in contact with him occasionally and he is just the right type.' And that is the way Dr. Frederick M. Becket impresses everybody. The right type. Most Institute members of the western group of hard-rock minors do not know him, but then they meet him in his swing around the circle next year they will not require a long acquaintance to sense his kindly and outstanding personality, to realize that he is a gentleman in the bet meaning o1 that word, a man of wide sympathies and interests.

Jan 1, 1932

Year Institute of Metals ? Petroleum - Iron and Steel ? Coal ? Mineral Industry Education - Industrial Minerals 1918 W M CORSE 1919 1920 W H BASSETT 1921 1922 W B PRICE 1923 E DEGOLYER 1924 G K ELLIOTT 1925 F JULIUS FOHS 1926 PAUL D MERICA 1927 JOHN M LOVEJOY 1928 S SKOWRONSKI A W AMBROSE RALPH H SWEETSER 1929 J B UMPLEBY G B WATERHOLSE 1930 ZAY JEFFRIES C V MILLIKAN W J MACKENZIEHOWARD N EAVENSON 1931 SAM TOUR C E BEECHER F M BECKET 1932 C H MATHEWSON EARL OLIVER F N SPELLERTHOMAS G FEAR C H FULTON

Jan 1, 1952

Albert Arents, Alameda, Cal.: From Mr. Furman's description of his crucible-assays I infer that he regards iron nails as a necessary or advisable adjunct. Against such a notion I must beg leave to protest. Nails should not be used in

Jan 1, 1896

Extremes in temperature and weather, along with the highly corrosive nature of acid leach solutions used at open-pit copper mines, necessitates the use of pipeline systems that are both corrosion resistant and impervious to the environment.

Jan 6, 1976

By K. M. Rolls, J. Wulff, D. A. Colling

Solid-solution alloys of the Ta- Ti system containing up to 70 at. pct Ti were melted and fabricated into wire. Steady magnetic-field measurements of cold-worked wires at 4.2°K indicate that the resistive critical field increases smoothly with increasing titanium, reaching a maximum of 93 kG (J = 1 amp per sq cm) for a composition of about 50 at. pct Ti. The composition dependence of the resistive critical field indicates it is largely paramagnetically limited for alloys containing more than 35 at. pct Ti. For cold-worked wires the value of the critical current density, Jc , was found to be insensitive to composition changes for compositions in excess of 20 at. pct Ti. It was observed that Jc could be increased by final-size heat treatment at 400°C without altering the value of- the resistive critical field. Experimental data are used to calculate the electronic specific-heat coefficient and the "upper critical field" for the alloys studied. THE effect and importance of metallurgical structure on superconducting properties have been summarized by Livingston and Schadler.1 Specific work on solid-solution alloys such as Nb-zr2-7 and Nb-Ti5-7 have shown that critical current density (Jc) and superconducting transition temperature are structure-sensitive. Berlincourt et al.6,8,9 in their studies of transition-metal alloys find that Ta-Ti alloys remain superconducting at fields comparable to Nb-Ti alloys. 6,8 Transverse critical current tests of a Ta-10 at. pct Ti alloy10 and longitudinal critical current tests of a Ta-25 at. pct Ti alloy1' indicate that such alloys are capable of carrying high currents at intermediate fields (-40 kG). The work reported in the present paper was undertaken to explore the superconducting properties of further compositions in the Ta-Ti alloy system as well as the structure sensitivity of the superconducting properties. I) EXPERIMENTAL PROCEDURE Alloys were prepared by melting tantalum (Fansteel Metallurgical Corp., 99.96 pct purity) and iodide, crystal bar titanium (Foote Mineral Co., 99.92 pct purity) mixtures in an arc furnace on a water-cooled copper hearth using a tungsten electrode. Melting was accomplished in a purified, gettered argon atmosphere at pressures from 250 to 400 Torr. Each alloy was turned and remelted fourteen times to assure complete mixing of tantalum and titanium. Ex- cessive coring in the cast samples was, nevertheless, observed. This was somewhat reduced by annealing in vacuo at 1000°C for 13 hr. The ingots were then machined to 0.250 in. diam, jacketed in Type 304 stainless-steel tubing, and swaged to 0.140 in. diam. They were then drawn to 0.010-in.-diam wire. Alloys containing up to 70 at. pct Ti were readily cold-drawn to wire in this manner. Later experiments showed that oxygen additions up to -3000 ppm could also be cold-worked into wire. Test samples for superconductivity measurements in the 2-in, air-core Bitter solenoids of the M.I.T. National Magnet Laboratory were prepared from 10-in. lengths of 0.010-in.-diam wire, cleaned of residual wire-drawing lubricant. Current contacts were made by clamping clean copper tubing over both No. 18 current lead wire and the ultrasonically indium-tinned ends of the specimen wire.12 Potential leads of No. 32 copper wire were connected to the specimen by ultrasonic soldering in an indium bath. The potential lead separation was about 4 cm, corresponding to the circumference of the Bakelite rod to which the wire was affixed with half-mil Teflon tape. The final specimen configuration is shown in Fig. 1. Specimens were lowered into a liquid helium bath (4.2oK) in a double solenoid dewar and positioned so that the maximum magnetic field was oriented transverse to the wire axis of the gage section. Measurements were made by passing a current through the specimen at a preset solenoidal magnetic field. The current was increased until a 1-pv potential difference appeared across the gage section (1/4 µv per cm). At low magnetic fields, however, it was not possible to use this criterion because power-dissipation difficul-

Jan 1, 1967

By E. A. von Hahn, T. R. lngraham

The rates of cementation of pd11 on electropolislzed copper cylinders were studied in aqueous perchloric acid solutions at pdII concentrations from 0.02 to 0.1 mM. The cylinders were rotated at various high speeds to reduce the diffusion layer to a minimum thickness. In 0.1 M HClO4 solutions, the cemented palladium is dense, adherent, and shiny. The rate data indicate that there are two stages in the deposition. In the initial stage, the rate of cementation is first order with respect to the pd11 concentration. The second stage is much slower. The first stage is consistent with rate control by the diffusion of pd11 ions to the copper surface, and/or chemical reaction at the surface, and the second stage is consistent with rate control by the diffusion of copper ions from the cop-per surface through the deposit of cemented palladium, out to the main body of solution. In 0.001 M HClO4 solution, only the first stage is evident and the rate is more rapid than at higher acidities. This rate enhancement is attributed to PdOH+ ions that predominate at low acidity and aye more reactive than unhydrolyzed pdII. The deposit is porous and loose. All of the cemented deposits are Pd-Cu alloys rather than pure palladium. Activation energies are 9.5 kcal per mole in 0.1 M HClO4 and 7.4 kcal per mole in 0.001 M HClO4. CEMENTATION or displacement reactions occur between aqueous solutions of metal salts and immersed metals according to the general equation: where M1 is electrochemically the more noble metal. Although these reactions find considerable application in metals recovery processes (e.g., the cementation of copper192 or gold3), in electrorefining processes (e.g., solution purification before electrolysis4,5), and in plating and metal finishing processes,6 few studies have been made of the kinetics of such reactions.7-9 The rates of cementation reactions will depend on one or more of the following factors: a) chemical reactions at the metal-solution interface; b) ionic transport to or away from the interface;'-' and c) the character and adherence of the cemented deposit on the substrate metal,6a,10 because the deposit will inhibit the rate of transport of dissolving ions (M2m+) into the solution. In this investigation, the kinetics of the early stages of cementation were studied to obtain an understanding of the reaction mechanism under conditions in which the deposit was sufficiently thin that its inhibiting effect could be disregarded. To achieve this, very dilute solutions in Mn+ were used. Cementation rates are often fast in the initial stages and transport-contr01led.9 To find conditions under which transport control would shift to chemical control, very high stirring velocities were used to minimize the diffusion-layer thickness. Of the many possible cementation reaction systems, the palladous perchlorate-copper system was chosen for this investigation because it was believed to involve simple ion-for-ion exchange. In addition, there are no interfering side reactions, such as the reduction of hydrogen ions, and anion effects are usually absent in perchlorate solutions. EXPERIMENTAL Materials. Reagent-grade chemicals and redistilled water were used in all experiments. Palladous perchlorate stock solutions (0.02 M) were prepared by dissolving 99.5 pct Pd sponge (Johnson Matthey and Mallory Ltd.) in concentrated nitric acid, adding concentrated perchloric acid, evaporating twice slowly (to prevent PdO precipitation) to a small volume, and diluting in a volumetric flask. To prevent gradual hydrolysis of PdII, the stock solutions were made 0.4 M in HC104. Tests for pdIV (Ref. 11) and C1- were negative. Copper strips were cut accurately from 0.025-in. electrolytic tough pitch sheet, Sample 1 (Mines Branch stock or Canadian Copper Refineries Ltd., Montreal), or from oxygen-free, high-conductivity sheet, Sample 2 (American Metal Climax O.F.H.C. brand, sold by Utility Brass and Copper Corp., Brooklyn). The strips were annealed for 1 hr at 335°C in a stream of purified nitrogen (Union Carbide, Linde Division) which had

Jan 1, 1967

The United States has never been a large coal exporting nation, and normally such shipments, aside from those to Canada, have been relatively small. Since the first railroad was built across the Allegheny Mountains, the imports have been quite small also, although fairly large tonnages of Canadian coal have moved into the extreme northeastern and northwestern states at times. In Table 21 are shown all data available about these shipments from 1790 to 1939, inclusive.

Jan 1, 1942

By Robert D. Pehlke, Robert G. Blossey

The solubility of nitrogen in liquid cobalt and a number of dilute cobalt alloys Was measured in the temperature range 1550" to 1700°C at nitrogen pressures to 1 atm. At 1600°C and 1 atm nitrogen pressure, the solubility in pure cobalt is 0.0047 wt pct [3.8 cu cm (stp) per 100 g Co]. The standard free- energy change for the solution reaction 1/2 N,(g) = gout pct in Co) is iF - 10,000 + 5.24 T cal per g atom N. The alloying elements Cv, Cu, Mo, Nb, Tu, W, and V increase the nitrogen solubility, while Al, Fe, Ni, and Si decrease the nitrogen solubility. THE solubility of nitrogen in cobalt was studied previously by Sieverts, Busch and Dodd,2 and Schenck, Frohberg, and Graf.3 Sieverts investigated the solution below the melting point of cobalt, and Busch and Dodd worked with the liquid metal; however, neither study found any solubility for nitrogen in cobalt. Schenck et al, reported a solubility of 0.005 wt pct N in cobalt at 1600°C. Seagle et al. 4 reported residual nitrogen in cobalt after electron-beam melting, although no reasons were ventured for the presence of this interstitial impurity. This investigation was undertaken to clarify these inconsistencies, and to provide additional data on atomic interactions in dilute metallic solution. EXPERIMENTAL PROCEDURE This study was well-suited to the Sieverts' method, which has not changed significantly since its introduction by Sieverts. 5 The apparatus was of the same design as that described by Humbert and Elliott, 6 with a reaction bulb similar to that reported by Weinstein and Elliott. 7 The buret was not water-jacketed, but the measured gas volumes were corrected for small changes in room temperature. The melt temperature was measured by a disappear ing-filament optical pyrometer sighted through a prism onto the melt surface. Temperature calibration was made based on a measurement of the melting point of pure cobalt taken as 1495°C. The difference between the reciprocal of the observed and the true temperatures was assumed to be a constant, neglecting the changes in emissivity with small additions of alloying elements. The total error in gas-volume measurement caused by accuracy limitations in reading the mercury level in the buret, variation in ambient temperature, and variation in melt temperature was about 0.5 cu cm. This represents approximately 10 pct of the total solubility, and is a larger relative error than in previous studies6-' because of the small nitrogen solubilities encountered in the present investigation. The source and purity of the materials used are listed in Table IA. Recrystallized alumina crucibles were used throughout the investigation. Examination of the crucibles after solidification of the melts showed no reaction or penetration. Alloying of the cobalt melt was accomplished with the dropping technique described by Humbert. 6 The investigation was started using cobalt from African Metals Corp. in shot form, but this material was not of sufficient purity and did not yield consistent solubility results. Sherritt Gordon Mines Ltd. cobalt was then used throughout the investigation. In experiments involving alloying elements which could react with oxygen dissolved in the melt, the cobalt was further refined by annealing at 1400°C in a dry-hydrogen atmosphere. This treatment, described by Woolley and Pehlke, 8 markedly reduced the oxygen content. The oxygen and nitrogen analyses of the cobalt used in this study are presented in Table IB. RESULTS Hot Volume. The hot volume was measured prior to each run and was 50 to 55 cu cm (stp) at 1600°C. It increased linearly with increasing pressure and decreasing melt temperature. Pure Cobalt. Measurements of the solubility of nitrogen in pure cobalt and the temperature coefficient of solubility are summarized in Table 11. At 1600°C and 1 atm nitrogen pressure, the solubility was found

Jan 1, 1967

By AIME AIME

0 N March 5, at Carnegie Hall, Cleveland, the Ohio Section held a joint meeting with the Cleveland Engineering Society, and the local sections of the American Chemical Society, American Society of Mechanical Engineers, and the American Society for Steel Treating. Prior to the meeting there was an informal dinner attended by 50 men. Then followed an address, "The Principles of Corrosion Protection," by Ulick R. Evans, the well-known British specialist in this problem. There were 266 present, presided over by Zay Jeffries, president of the American Society for Steel Treating and a member of the Cleveland Engineering Society. The address was well received and some discussion followed

Jan 1, 1929

By B. W. Levinger

THE lattice parameter of the ß form of pure titanium has been measured at elevated temperature.', ' No attempt was made, however, to correct the parameter obtained to room temperature. In the course of phase diagram studies at Armour Research Foundation and elsewhere, the variation of ß-phase lattice parameter with composition has been established in a number of binary and ternary systems involving titanium. It was possible to extrapolate in these instances to 100 pct Ti to find the apparent lattice parameter of ß titanium at room temperature. Table I lists the results thus obtained. The suggested value for the lattice parameter of ß titanium is the average of the extrapolated values 3.276 ±0.003 kX. This suggested value gives an interatomic distance in ± titanium of 2.837 kX and hence a Goldschmidt atomic diameter (coordination number 12) of 2.925 kX. The latter agrees closely with the value of 2.93 given by Hume-Rothery." From the data of Adenstedt and coworkers' it was possible to determine by extrapolation the mean coefficient of linear expansion for /3 titanium in the range from room temperature to 1000°C. This value, 10.1x10-8 per degree C, compares with about 11x10-8 for a titanium in a similar range." It was thus possible to calculate the parameter at 900 °C. The value of 3.305 kX agrees well with 3.3065 given by Eppel-sheimer.' The majority of values reported in the literature7-', ' were given as Angstroms. In at least one case, ref. 8, it was shown that they actually represented kX units. The source of this confusion appears to be that a large number of tables of X-ray emission spectra list wavelengths as Angstroms and give values in kX units. The accepted conversion factor for kX units to Angstroms (10.' cm) is 1.00202. Thus the parameter of ß titanium suggested corresponds to 3.282A. References J. H. de Boer, W. G. Burgers, and J. D. Fast: Proc. Acad. Amsterdam (1936) 39, p. 515. 2D. S. Eppelsheimer and R. R. Penman: Nature (Dec. 2, 1950) 166, p. 960. 3 W. Hume-Rothery: The Structure of Metals and Alloys (1945) London. Inst. Metals. 4 H. K. Adenstedt, J. R. Pequignot, and J. M. Raymer: Trans. ASM (1952) 44, p. 990. 5 Gmelins Handbuch der Anorganischen Chemie. Titan, Verlag Chemie, Weinhein (1951). 8 P. Pietrokowsky and P. Duwez: Trans. AIME (1952) 194, p. 627; Journal of Metals (June 1952). 7 P. Duwez and J. L. Taylor: Trans. ASM (1952) 44. D. 495. 8 M. Hansen, E. L. Kamen, H. D. Kessler, and D. J. McPherson: Trans. AIME (1951) 191, p, 881; Journal of Metals (October 1951). 8 Unpublished Research, Armour Research Foundation.

Jan 1, 1954

By H. L. Gilbert, W. W. Stephens

Production of anhydrous zirconium tetrachloride by direct chlor- ination of a zirconium oxide carbon mixture in a silica-brick-lined chlorinator is described. Theory and thermodynamics of reactions are discussed. A pilot-model chlorinator and full-scale production equipment are described and operating data are included. ANHYDROUS zirconium tetrachloride required as a starting material in the Kroll process for production of ductile zirconium has been produced in this country principally by chlorination of the carbide or "carbonitride" made by reduction of zircon sand concentrates with carbon in the arc furnace. This process and the equipment used have been fully described.'.' It is well known that zircon or badde-leyite ores may be chlorinated directly with chlorine in the presence of carbon, and this one-step approach would seem at first glance to be preferable to the two steps involved in the carbide-chloride operation. As previously discussed1 considerations leading to adoption of the longer process were: 1—Chlorination of the carbide proceeds rapidly at temperatures below 500°C, whereas temperatures above 900°C were considered necessary for chlorination of zircon-carbon mixtures. 2—The highly exothermic nature of the carbide-chlorine reaction makes it self-sustaining, while heat must be supplied continuously in direct chlorination of the ore. 3—Silicon was thought to be chlorinated along with zirconium in the direct chlorination of zircon, leading to high chlorine consumption. In production of carbide in the arc furnace, silicon is driven off as silicon monoxide and does not enter the chlorinator. 4—For efficient direct chlorination, the ore must be finely ground and intimately mixed with carbon, and the mixture briquetted. 5—Direct chlorination requires a much larger chlorinator for a given production capacity than chlorination of carbide. Recently it has become necessary to produce large quantities of zirconium metal from a chemically purified zirconium oxide. Since the cost of the latter is high, the relatively high losses encountered in production of carbide in the arc furnace could not be tolerated, and a graphite resistor furnace5 was developed for production of carbide, which was then chlorinated in equipment previously used for chlorinating arc-furnace carbide. This method of operation was quite satisfactory, and losses in the carbid-ing step were minimized. However, operating costs were relatively high, and the process did not lend itself particularly well to large-scale operation because of the multiplicity of small units required and the hand labor needed to load, unload, and maintain the furnaces. To chlorinate the carbide, a vertical-shaft chlorinator was used in which the charge was heated with a central split graphite-rod resistor.' Operation of this chlorinator was somewhat less satisfactory with the resistor furnace carbide than it had been with the arc-furnace carbide due, principally, to the differences in physical properties of the carbide. The arc-furnace carbide is obtained as a fused metallic-appearing mass which can be crushed to -1/4 in. with production of a minimum of fines, whereas the resistor-furnace product is lightly sintered and produces a large proportion of fines in crushing and handling. These fines tend to pack in the chlorinator and promote channeling. which results in poor chlorine efficiency and low capacity. Data based on production of 22,000 lb of chloride from resistor-furnace carbide in this equipment are shown in Table I. Necessity for increasing production of chloride from about 2,000 to 15,000 lb per week led to further investigation of possible methods for direct chlorination of the oxide or oxide-carbon mixtures. Direct chlorination of the pure oxide presents much less difficulty than chlorination of zircon sand or oxide ores. The oxide is easily ground to —200 mesh, and no silica is present to cause excessive consumption of chlorine or contamination of the product. Theoretical Considerations The principal chemical reactions involved in chlorination of mixtures of zirconium oxide and carbon may be written as follows: ½ ZrO2 (c) + C(c) + Cl2(g) = ½ ZrCl,(g) + CO(g) [I] 1/2 ZrO, (c) + CO(g) + Cl2(g) = ½ ZrCl,(g) + CO2(g) 121 ½ ZrO2 (c) + ½ C(C) + Cl2(g) = 1/2 ZrCl4(g) + ½ CO2(g) [3]

Jan 1, 1953

By Alan Stanley

THE Maclntyre Development of National Lead Co. is located at Tahawus, N. Y., in the heart of the Adirondack Mountains. Operations involve the mining and concentrating of a titaniferous iron ore to produce ilmenite and magnetite concentrates. A general description of the operation and metallurgy has been given by Frank R. Milliken.1 Pigment plant production demands that the MacIntyre mill produce a 44.7 pct. TiO2 ilmenite concentrate. To achieve the required ilmenite grade and tonnage it is important that the table concentrate grade be closely controlled. Unfortunately, however, the titaniferous orebody which feeds the Maclntyre mill is not uniform. Ore dressing characteristics vary from one end of the orebody to the other, and from one level to the next.. The changeable nature of the mill feed precludes a single adjustment of the equipment for long periods of time. Thus the operators must constantly watch the equipment to insure a uniform concentrate from the fine and coarse tables and Wetherills, or dry magnetic separators. Chemical assaying of mill products requires about 4 hr from the time the sample is taken until assay results are obtained, and this is available only on a two-shift basis. The ore may change rapidly, even several times during a shift, so that assay results lose most of their control value by the time they are reported to the mill operating crew. Members of the crew have therefore tried to evaluate the table and Wetherill concentrate by visual inspection, since through long experience the shift operators, under most circumstances, can gage closely the grade of the mill products. However, there are times when the, physical nature of the ore is radically different from normal. Under these conditions visual inspection is of no value, and at such times final ilmenite as low as 43 pct TiO2 has been produced and shipped before the assay results have been received. The specific gravity method of assaying for TiO2 has been attempted to eliminate the shipping of ilmenite below normal grade as well as to help control day to day and hour to hour mill production. Table I shows the minerals found in the Maclntyre ore along with their average weight proportions and specific gravities. The first two products considered for the specific gravity method were fine and coarse table concentrates. It was reasoned that these products were essentially ilmenite with the higher specific gravity gangue minerals. Since they were always produced the same way, and the desired grade of TiO2 was always constant, the specific gravity of these materials would increase or decrease as the amount of ilmenite increased or decreased. Thus for table concentrates which assayed 40 pct TiO2 a constant gravity would invariably be obtained, and as the TiO2 value changed the specific gravity would change in direct proportion. The third product considered was Wetherill ilmenite. It was assumed that a desired grade of 44.7 pct TiO2 would also always contain the same amount and type of gangue minerals along with the ilmenite, and thus would always have the same specific gravity. As the TiO2 value of the ilmenite concentrate changed so would its specific gravity. Dr. Kenneth Vincent, chief metallurgist of the Baroid Division of National Lead Co. at Magnet Grove, Ark., ran specific gravity tests on 17 samples of the desired products. The lowest specific gravity reading assayed the lowest in TiO2 and as the specific gravity increased the trend was for the TiO2 assay to increase, see Fig. 1. Since these results warranted further investigation, a 500-g capacity Torsion balance and 250 ml Le Chatelier specific gravity bottles were obtained. [ ] Shift samples of fine table concentrate, coarse table concentrate, and final ilmenite were tested. Each sample was split and 85 g weighed on the Torsion balance. The Le Chatelier bottle was filled with water to a zero mark. To avoid wetting the neck of the bottle it was found necessary to do this

Jan 1, 1952

By Alan Stanley

THE MacIntyre Development of National Lead Co. is located at Tahawus, N. Y., in the heart of the Adirondack Mountains. Operations involve the mining and concentrating of a titaniferous iron ore to produce ilmenite and magnetite concentrates. A general description of the operation and metallurgy has been given by Frank R. Milliken.' Pigment plant production demands that the MacIntyre mill produce a 44.7 pct TiO, ilmenite concentrate. To achieve the required ilmenite grade and tonnage it is important that the table concentrate grade be closely controlled. Unfortunately, however, the titaniferous orebody which feeds the MacIntyre mill is not uniform. Ore dressing characteristics vary from one end of the orebody to the other, and from • one level to the next. The changeable nature of the mill feed precludes a single adjustment of the equipment for long periods of time. Thus the operators must constantly watch the equipment to insure a uniform concentrate from the fine and coarse tables and Wetherills, or dry magnetic separators. Chemical assaying of mill products requires about 4 hr from the time the sample is taken until assay results are obtained, and this is available only on a two-shift basis. The ore may change rapidly, even several times during a shift, so that assay results lose most of their control value by the time they are reported to the mill operating crew. Members of the crew have therefore tried to evaluate the table and Wetherill concentrate by visual inspection, since through long experience the shift operators, under most circumstances, can gage closely the grade of the mill products. However, there are times when the physical nature of the ore is radically different from normal. Under these conditions visual inspection is of no value, and at such times final ilmenite as low as 43 pct TiO, has been produced and shipped before the assay results have been received. The specific gravity method of assaying for TiO, has been attempted to eliminate the shipping of ilmenite below normal grade as well as to help control day to day and hour to hour mill production. Table I shows the minerals found in the MacIntyre ore along with their average weight proportions and specific gravities. The first two products considered for the specific gravity method were fine and coarse table concentrates. It was reasoned that these products were essentially ilmenite with the higher specific gravity gangue minerals. Since they were always produced the same way, and the desired grade of TiO, was always constant, the specific gravity of these materials would increase or decrease as the amount of ilmenite increased or decreased. Thus for table concentrates which assayed 40 pct TiOz a constant gravity would invariably be obtained, and as the TiO, value changed the specific gravity would change in direct proportion. The third product considered was Wetherill ilmenite. It was assumed that a desired grade of 44.7 pct Ti02 would also always contain the same amount and type of gangue minerals along with the ilmenite, and thus would always have the same specific gravity. As the TiO, value of the ilmenite concentrate changed so would its specific gravity. Dr. Kenneth Vincent, chief metallurgist of the Baroid Division of National Lead Co. at Magnet Grove, Ark., ran specific gravity tests on 17 samples of the desired products. The lowest specific gravity reading assayed the lowest in TiO, and as the specific gravity increased the trend was for the TiO, assay to increase, see Fig. 1. Since these results warranted further investigation, a 500-g capacity Torsion balance and 250 ml Le Chatelier specific gravity bottles were obtained. Shift samples of fine table concentrate, coarse table concentrate, and final ilmenite were tested. Each sample was split and 85 g weighed on the Torsion balance. The Le Chatelier bottle was filled with water to a zero mark. To avoid wetting the neck of the bottle it was found necessary to do this

Jan 1, 1953