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Powder Metallurgy Committee Local Sections DETROIT Robert Henderson, President, Victor Gallatin, Vice-President, Secretary, J I Farmer, Treasurer John Check, NEW YORK K H Roll, Chairman

Jan 1, 1957

By C. M. Brinckerhoff

Safety work in mining at the Andes Copper Mining Company, Potrerillos, Chile, is divided into three parts: (1) accident prevention, (2) fire prevention and protection, and (3) silicosis prevention and control. In the company's operations a steady campaign has been waged to reduce accidents and silicosis, and to prevent fires. In the following pages the safety record for the past twelve years will be examined and the methods explained by which the accident rate was reduced. Table 1 contains yearly data pertaining to the scale of the mining operations and the accident record. Block caving is used for all ore production and the tonnage mined has averaged 30,000 short tons per day for the past seven years. Table 2 classifies 44 fatal accidents which have occurred since 1935. The leading causes of accidental death are transportation of ore and use of explosives, followed in order by persons falling, falls of ground, and by asphyxiation. In the case of serious accidents, however, the greatest cause is falls of ground, followed, in turn, by ore transportation, persons falling, explosives, and asphyxiation. Accident Prevention The improvement of the safety record was obtained by a combination of many factors. In surveying the results at Andes for the past twelve years, it is possible to select some features of the present operation which have contributed to the accident record. The most important of these are: (1) good staff planning, (2) good equipment, (3) an alert safety organization, and (4) education and selection of the workmen. GOOD STAFF PLANNING As a result of good staff planning, the mine has good working conditions, namely, good ventilation, moderate temperatures and humidity, and good lighting. These factors not only reduce accidents but also improve efficiency. In haulage work, accidents have been reduced by having traffic move in a forward direction only. The latter makes possible a one-man train crew. Trains are centrally dispatched from loading drifts which are interconnected by signal lights, so that when a train in a lateral drift is given permission to move into a main line drift, a red light signals in all other lateral drifts in that area. Good track is maintained, and safety niches are required at all switch throws. Since safety niches were provided there have been no fatal or serious accidents at such points. All main line haulage drifts are illuminated by electric lights. Haulage drifts are kept clean. Adequate clearance has been provided between cars and between cars and the sides of the haulage drifts. The 4 1/2 ton Cranby type cars are equipped with roller bearings, and the 10 ton loconlotives with trolley shoes instead of wheels. These two features are responsible for improved ore haulage conditions and contribute to greater efficiency and safety.

Jan 1, 1950

By T. Kusakawa

In Japan, natural gypsum is rarely mined for industrial use and almost all gypsum is synthetic, that is desulphogypsum, produced from waste sulphur dioxide gas from metal smelters and power plants and other industrial waste sources. The amount of synthetic gypsum production (1979) reached more than 6 Mt/a (6.6 million stpy). Major uses are for cement and building materials. Other uses include soil conditioner, investment casting molds, and organic composite materials. Sulphur recovery by gypsum decomposition is being examined. This paper summarizes present Japanese production and uses of synthetic gypsum produced from industrial wastes.

Jan 1, 1984

By Marcus A. Grossman

THE institute has established this lectureship to honor the memory of a great American metallurgist, one whose fame has continued long after his passing. As one scientist recently stated it," All metallurgical texts gradually become outdated and outmoded, except those of the great Henry Marion Howe." It seems fitting, then, that, once every year, we should review, in his honor, some aspects of the science in which he was such a distinguished leader, and also discuss any new data that may help to clarify our concepts. It is my privilege, for which indeed I express the deepest appreciation to this Institute, to offer for consideration a few thoughts on the toughness and fracture of hardened steels. Before proceeding to the data, I wish to express my great indebtedness to many associates whose stimulating discussions, generous contributions of data and cooperation in experiments are gratefully acknowledged. (But I wish to absolve them of any blame that may arise from the way in which their discussions and data have been used!) First, Dr. Edgar C. Bain, Vice President, Carnegie-Illinois Steel Corporation, whose amiable but merciless criticisms and always constructive and thoughtful suggestions help unfailingly to guard against pitfalls. Then to associates at Gary Steel Works, especially Mr. H. B. Wishart, Mr. W. K. Smith and Mr. V. Elliott, for great assistance in securing data. Also to Col. C. H. Greenall, Director of Laboratories, Frankford Arsenal, and his metallurgical staff, including Messrs. J. K. Desmond, H. Markus, D. F. Armiento, H. Rosenthal and Henry George, for numerous data and illustrations. Further to Dr. J. R. Low and Dr. M. Asimow, for helpful discussions of effects of states of stress during deformation and rupture, to Mr. J. M. Hodge for discussions and data, to the staff of the U. S. Steel Corporation Research Laboratory for advice and data, and to the Metallurgical Staff at Duquesne Steel Works. The individual acknowledgments will also be found under illustrations. Acknowledgment is also due to Mr. S. C. Snyder for incredibly meticulous scrutiny of manuscript. To all of these, grateful thanks.

Jan 1, 1946

By Paul M. Tyler

MINOR industrial minerals included in this chapter are: the alum minerals, bromine, calcium chloride, epsomite and other natural magnesium salts, iodine, meerschaum, quartz, industrial crystals other than quartz (Iceland spar, tourmaline, fluorite, selenite, mica), and nonfuel gases (air, helium, carbon dioxide). ALUM MINERALS The alums comprise a series of double sulphates (or selenates) isomorphous with potash alum, which, according to a ruling of the Pennsylvania courts, is the only product commercially described simply as "alum." Common alum occurs in nature as kalinite (K2SO4- A12 (SO4) 324H2O). The mineral mendozite (Na2S04) 3.A12 (SO4)3- 24H2O) is soda alum; tschennigite (NH4)2SO4.Al2 (SO4)3.24H2O) is ammonium alum; and there are about a dozen other native alums and related double sulphates. Alunite (alumstone or alum rock) has the formula Al2(SO4) 3.K2S04.4A1 (OH)3 and alunogen, Al2(So4) 3.18H20. Saline residues, found wherever natural water is evaporated, may contain sulphate of alumina, which for most uses is the essential ingredient of alum. Mineral wells and springs that emerge from beds of pyritiferous shale are typically astringent and at times form local deposits of alum, generally as incrustations. Acid waters acting upon aluminous rocks may form sulphates of alumina. The alums of commerce, as well as aluminum sulphate (concentrated alum), are produced principally by treating bauxite with acid, but they have been made also on a substantial scale from clay, cryolite, pyritic slates, schists, lignites, alunite, and leucite. Alum shale-chiefly clay, pyrite, and (usually) carbonaceous matter-was extensively used in England as a source of alum for more than two centuries. In France, pyritic lignites mixed with sand and clay were burned in heaps to red ash, the leach Liquors from which, after treatment with ammonia, yielded alum and copperas. Processes have been developed for making alum or aluminum sulphate from such diverse materials as feldspar, aluminous phosphate minerals, greensand, and mixtures of mica and

Jan 1, 1949

[A Aall, Christian H., M49 A Dir, Smelt & Ref, Am. Metal Climax, Inc., 1270 Ave. of the Americas, New York 20, N. Y. Aaroe, S. L., A54 A VP, W. S. Tyler Co. of Canada Ltd., P. O. Box 100, St. Catharines, Ont., Canada Abalos, Teodulo Q., J57 A Prod Frmn, Lepanto Cons. Mining Co., Lepanto, Mt. Province, Philippines Abbitt, James M., A54 770 Sole Blvd., Bartow, Fla. Abdullah, M. Y., J53 Dept. of Mines Res. Div., P. O. Box 1016 Tiger Lane,-Ipoh Peram, Malaya Abel, John F., Jr., J53 F Mine Engr, Thompson Creek Coal & Coke, Carbondale, Colo. Abell, Leo M., M31 B Const Supt, Phelps Dodge Corp., Morenci, Ariz. Abendroth, H. E., A57 Mangore Australia Pty. Ltd., 901 Hay St., Perth, W. Aust.,, Australia Abenius, Hakan V., M52 Falun, Sweden]

Jan 1, 1961

By AIME AIME

THIS year the Chairman of the Institute's Iron and Steel Division is THIS William Anderson Haven, better known to the membership generally as Bill Haven. The Division Chairman is an individual endowed with a broad perspective of the ferrous metal industry he result of his earlier experiences as a successful operating man in the working and management of blast furnaces and his later experiences as an engineering-consulting executive concerned with the design and erection of and steel works throughout the world. William A. Haven was born to iron steel in the Pittsburgh district on ;. 1, 1888, and in due time--or in 1909 graduated from Penn State with a Bachelor degree in industrial chemistry.

Jan 1, 1944

By W. Smith, F. G. Rinker, D. Beggs

Early in 1965 the Surface Combustion Division of the Midland-Ross Corporation was awarded the contract to engineer and construct a taconite pelletizing plant for the National Steel pellet plant, administered by the Hanna Mining Co., near Keewatin, Minn. This plant, which will have an annual capacity of 2,400,000 long tons, will produce pellets from magnetite concentrate using a new process developed through a joint research program by Midland-Ross, Hanna Mining, and the National Steel Corp. The work that culminated in the decision to construct this plant is the result of a research program for the development of the Midland-Ross heat fast process for the production of prereduced or metallized pellets. PELLETIZING PROCESS There are many acceptable methods for producing oxide pellets from ground iron ores and concentrates, and all of these give an acceptable product for blast furnace utilization. The vertical shaft furnace, the traveling grate, and the grate-kiln have been installed in many pelletizing plants in the northern hemisphere; therefore, the acceptance of these methods and the problems associated with them are well understood. However, this research project investigated a method for improving upon these processes to produce a high quality oxide pellet at a low operating cost.

Jan 9, 1966

By A. H. Lee

Discussion of the paper of H. P. HOWLAND, printed in Bulletin No. 111, March, 1916, pp. 627 to 650. A. H. LEE, Buffalo, N. Y. (communication to the Secretary*). The statements and results recorded in Mr. Howland's paper can be accounted for by the use of coke with a low sulphur content (0.60 and under). This allows the furnaces to be run on a small volume of acid slag, which it is presumed was done in Mr. Howland's practice. H. A. Brassert has admitted that this was the largest factor in low fuel consumption in his practice. Where the coke contains from 1.00 to 1.25 per cent. of sulphur the situation is quite different and I doubt whether the results mentioned by Mr. Howland could be obtained under such circumstances. ` N. M. LANGDON, Mancelona, Mich. (communication to the Secretary + ).-Gruner's ideal working (which is but a statement of the law first enunciated by Bell) as given in Gordon's Translation of Studies of Blast Furnace Phenomena, "supposes that the reduction of the oxide of iron is effected by the CO only, without intervention of solid carbon." This ideal, if reached, would mean theoretically perfect or 100 per cent. efficiency of reduction. The workings of the large number of furnaces as given in Bell's and Gruner's great works do not show that this standard of perfection ever was reached. This problem has been worked out by the writer for a number of furnaces, and his results, as well as those given by others, all show a failure to reach perfection. Some furnaces, however, approach nearer to perfection than others. The "ideal" as given by Gruner was not stated as a solved problem in blast-furnace practice, but as an ideal to the attainment of which furnace managers should strive. A study of the factors involved from every angle is interesting and instructive and the paper on this subject contributed by H. P. Howland is no exception to the rule. This article is fairly open to criticism, not because of the unique method of presenting the subject, but for the reason that, as the writer conceives, erroneous assumptions are taken which lead naturally to incorrect conclusions.

Jan 7, 1916

By Ednlund D. North

Discussion of the paper of Edmund D. North, presented at the Spokane meeting, September, 1909, and published in Bulletin No. 37, January, 1910, pp. 21 to 25. A. SCOTT REID, London, Eng. (communication to the Secretary*) :-As a constructor of several glass mine-models, I have read with much interest the description of the model of the Montana-Tonopah mine-workings by Edmund D. North. As an interchange of ideas and experience is always an advantage, and in view of the fact that such models are coming more and more into vogue, perhaps the following remarks on this subject may prove of interest to mining engineers generally and to Mr. North particularly. In the model of the Waihi gold-mine, New Zealand, which I constructed, a dust-proof case is used. The top, bottom, front, and two ends are of glass; the back only is of wood, painted a dull white, against which the mine-workings show very distinctly. Each mine-level is represented by a horizontal sheet of glass, supported on metal runners fixed to the uprights at each end of the case, in a manner similar to that described by Mr. North. The corner uprights are strengthened by having a metal band screwed to the inside face of each, to which the metal runners or supports for the sheets of glass are screwed in turn. The reason for having this additional strength is that as the mine is developed in depth, and fresh levels are opened, the increasing weight of the glass sheets, added to the model, caused the unsupported wooden uprights to bend slightly, so that the glass sheets-did not fit in with the desired nicety, and co-ordination was, to a considerable extent, lost. Strengthening the uprights in this manner is not important in models of mines in which only a few levels have been opened, or when the sheets of glass are small, but in the Waihi model there are 15 sheets of glass to be supported, and more to be added as development proceeds, and the weight is considerable.

May 1, 1910

By Raymond D. Sloan

Retaining third place in crude-oil production among the nation's oil-producing states, Oklahoma's output in 1942 totaled 137,792,000 bbl., a decline of 9.4 per cent from the previous year's total of 152,117,000 bbl. Production declined from an average of 403,000 bbl. daily in January 1942 to an average of 355,000 bbl. during December, a reduction of 48,000 bbl. daily (11.9 per cent) during the year. At the end of 1942 it would appear inevitable that the downward trend in production will continue in 1953 unless halted in the immediate future by greater than normal discoveries and development. To Jan. I, 1943, Oklahoma has produced 5,067,013,000 bbl. oil crude oil. Development and Exploration Development dropped abruptly in 1942, reflecting the lack of any sizable discoveries and the effect of the provisions of Federal Well Spacing Order M-68, which became effective in December 1941. In all, 1210 wells were drilled in 1942. This represents a decrease of 42.7 per cent from the 1941 total of 2110. Of the total wells completed, 553 (45.7 per cent) were oil wells with an average initial production of 443 bbl.; 102 (8.4 per cent) were gas wells with an average initial of 3,359,000 cu. ft.; and 555 (45.9 per cent) were dry. Although the number of completions declined sharply, the total of 320 wildcats completed (26.4 per cent of all wells) repre-sents a decrease of only 2.7 per cent from the previous year's figure of 329. Of the wildcats drilled, 44 (13.8 per cent) were oil wells, 13 (4.0 per cent) were gas wells, and 263 (82.2 per cent) were recorded as failures. Reconditioning of wells throughout the state resulted in a total recompletion of 355 wells. Of these, 234 were oil wells with a combined initial production of 96,808 bbl., 32 were gas wells with a total initial of 381,488,000 cu. ft., and 89 were abandoned. None of the 26 pools found in 1942 has developed into a major discovery. The Pauls Valley pool, Garvin County, is the most outstanding. Since its discovery in April, 14 wells with an average initial of 1898 bbl. have produced 803,000 bbl. of 42' gravity oil from the Bromide zone. Development in this pool is believed to be almost completed. Other of the more important discoveries are the East Watchorn pool, Pawnee County; Guthrie Townsite and West Navina, Logan County; Brooksville and Macomb, Pottawatomie County, and the Liberty and Northeast Lucien discoveries in Noble county. The East Watchorn pool, at the close of the year, had 14 completed oil wells with an average initial of 989 bbl. from the Wilcox sand at 3930 it.; Guthrie Townsite, one well with an initial of 840 bbl. from dolomite at 5600 It.; West Navina, six wells with an average initial of 284 bbl. in the Lay ton sand at 5050 ft., Brooksville, eight wells in the Hunton at 4800 ft. with an average initial 01 355 bbl.; Macomb, one well with an initial of 160 bbl. in the IIunton at 4700 ft.; the Liberty pool, one well with an initial of 1268 bbl. in the second Wilcox at 4500 ft., and two wells in the Tonkawa sand at 2500 ft., with an average initial of 230 bbl. In the Northeast Lucien pool, four wells were completed in the Wilcox at 5380 ft. for an average initial of 1164 bbl., and one well was completed in the Viola lime at 5255 ft. for an initial of 55 barrels.

Jan 1, 1943

By Raymond D. Sloan

Retaining third place in crude-oil production among the nation's oil-producing states, Oklahoma's output in 1942 totaled 137,792,000 bbl., a decline of 9.4 per cent from the previous year's total of 152,117,000 bbl. Production declined from an average of 403,000 bbl. daily in January 1942 to an average of 355,000 bbl. during December, a reduction of 48,000 bbl. daily (11.9 per cent) during the year. At the end of 1942 it would appear inevitable that the downward trend in production will continue in 1953 unless halted in the immediate future by greater than normal discoveries and development. To Jan. I, 1943, Oklahoma has produced 5,067,013,000 bbl. oil crude oil. Development and Exploration Development dropped abruptly in 1942, reflecting the lack of any sizable discoveries and the effect of the provisions of Federal Well Spacing Order M-68, which became effective in December 1941. In all, 1210 wells were drilled in 1942. This represents a decrease of 42.7 per cent from the 1941 total of 2110. Of the total wells completed, 553 (45.7 per cent) were oil wells with an average initial production of 443 bbl.; 102 (8.4 per cent) were gas wells with an average initial of 3,359,000 cu. ft.; and 555 (45.9 per cent) were dry. Although the number of completions declined sharply, the total of 320 wildcats completed (26.4 per cent of all wells) repre-sents a decrease of only 2.7 per cent from the previous year's figure of 329. Of the wildcats drilled, 44 (13.8 per cent) were oil wells, 13 (4.0 per cent) were gas wells, and 263 (82.2 per cent) were recorded as failures. Reconditioning of wells throughout the state resulted in a total recompletion of 355 wells. Of these, 234 were oil wells with a combined initial production of 96,808 bbl., 32 were gas wells with a total initial of 381,488,000 cu. ft., and 89 were abandoned. None of the 26 pools found in 1942 has developed into a major discovery. The Pauls Valley pool, Garvin County, is the most outstanding. Since its discovery in April, 14 wells with an average initial of 1898 bbl. have produced 803,000 bbl. of 42' gravity oil from the Bromide zone. Development in this pool is believed to be almost completed. Other of the more important discoveries are the East Watchorn pool, Pawnee County; Guthrie Townsite and West Navina, Logan County; Brooksville and Macomb, Pottawatomie County, and the Liberty and Northeast Lucien discoveries in Noble county. The East Watchorn pool, at the close of the year, had 14 completed oil wells with an average initial of 989 bbl. from the Wilcox sand at 3930 it.; Guthrie Townsite, one well with an initial of 840 bbl. from dolomite at 5600 It.; West Navina, six wells with an average initial of 284 bbl. in the Lay ton sand at 5050 ft., Brooksville, eight wells in the Hunton at 4800 ft. with an average initial 01 355 bbl.; Macomb, one well with an initial of 160 bbl. in the IIunton at 4700 ft.; the Liberty pool, one well with an initial of 1268 bbl. in the second Wilcox at 4500 ft., and two wells in the Tonkawa sand at 2500 ft., with an average initial of 230 bbl. In the Northeast Lucien pool, four wells were completed in the Wilcox at 5380 ft. for an average initial of 1164 bbl., and one well was completed in the Viola lime at 5255 ft. for an initial of 55 barrels.

Jan 1, 1943

By Milnor Roberts

WAR struck the mineral industry of Washington with cross currents that produced a peculiar result. The State's production of coal, industrial minerals, and metals for 1941, valued at $28,507,282, was increased in 1942 under war pressure to approximately $35.000,000. Meanwhile a tremendous demand had arisen for men to construct airfields and many other large projects for the Army and Navy in Washington and Alaska, and Government plants for the mineral industry costing $140,000,000 or more, as well as a call for employees in the U. S. Navy Yard at Bremerton, the sixty shipyards, the four Boeing airplane factories with many auxiliary shops, and hundreds of other plants turning out war materials. In spite of an influx of nearly 300,000 people, causing an increase of 17.1 percent in the population since 1940, according to the Census Bureau, the State clearly is still engaged in an unusual amount of war production in proportion to its population. A large proportion of the workers have been drawn from the mineral industry to the war plants, whether through motives of patriotism, high wages, or, in the Boeing plants at least, the glamour of the operation

Jan 1, 1944

Note by the Secretary.-—In the preceding communication of Mr. Rickard, in the present discussion, as printed in Trans., xxiii., the loss of quicksilver at Pestarena, reported on p. 569, as 230 and 234 grammes per metric ton, is stated as equivalent to about 74 pounds per short ton avoirdupois—an obvious error, which escaped correction in my reading of the proofs, and was not discovered until after Vol. XXIII. had left the press. The true equivalent is 0.46 pound or about 7 1/2 ounces (instead of pounds) per short ton.— R. w. R. Philip Argall, Denver, Colo. (communication to the Secretary) : Mr. Rickard's last contribution to this discussion* calls for some reply from me, if only by way of defending myself against the charge (p. 569) that my criticisms of his paper were "unnecessarily hypercritical and occasionally unfair." At the same time I am fully aware that our Transactions are not the place for mere personal controversy, and that the sole object of discussion is to define differences of opinion, and defend opposing views as a means of eliciting the truth. Mr. Rickard disclaims the statement, which he says I attributed to him, that in the slow-crushing Gilpin county mills the pyrites remain longer in the mortar than the other portions of the ore. My understanding of his statement was based on the following passages in his paper: " Particles of ore, which have heen pulverized to a fineness which would permit of their exit through the screen, are enabled to settle towards the bottom of the mortar. It would he expected that the heavy metallic minerals occurring in the ore would, because of their greater specific gravity, be most affected by this feature of the treatment. In practice this is found to be so. The fine slimes contain a large proportion of metallic sulphides, generally valuable on account of their close association with the precious metals, while the coarsest particles to be found in the tailings usually consist of quartz and other minerals forming the less heavy gangue (Trans., xxiii., 139).

Jan 1, 1895

By H. C. Johnson, J. K. Elliott

One of the primary requirements for successful operation of an enriched gas-drive project is to control the composition of injection gas. This can become a serious and difficult problem, particularly in cases where the enrichment material is being furnished from a number of field -produced gas streams. It is possible to effect control of the injection gas composition through frequent or continuous sampling; however, this can be extremely costly and, in many cases, impractical due to laboratory requirements of time. Another alternative would be to provide a calculation technique which would be flexible and sufficiently accurate to predict composition of the liquid and gas streams of interest at any point in the system. The purpose of this paper is to discuss a technique that was used successfully on an operating enriched gas-drive project for developing information which could be used for controlling composition of the injected gas. FIELD OPERATIONS The particular field (hereafter called Example field) in the example operation being discussed is composed of four oil reservoirs (A. B, C and E) and one gas condensate reservoir (D). Casinghead gas from the oil reservoirs and gas from the gas condensate reservoir are gathered through a field gathering system as shown in Fig. I for injection into Reservoir C. The gas mixture which is recovered from the five reservoirs for injection purposes is composed of gases liberated in 19 individual separators, each operating at a separate temperature and pressure. PROPOSED CALCULATION TECHNIQUE It is well known that vapor-liquid equilibrium calculations in general use throughout the petroleum industry can be used to predict reliably the phase behavior of hydrocarbon mixtures, particularly at pressures less than 1,000 psig. It is then a simple matter to account for the material on a ComPonent basis by m''ing flash and material balance calculations at each separation point in a hydrocarbon system. Accordingly, it was proposed to use vapor-liquid equilibrium and material balance cal- culations with a medium-sized electronic digital computer as a basis for developing a control procedure for use in controlling injection gas composition in the enriched gas-drive project. Although the approach is a simple one, the numerous vapor-liquid equilibrium calculations involved make the problem laborious; in this particular case, it would have been impractical to make sutficiently complete analysis without the aid of digital computing equipment. SAMPLING AND VERIFICATION OF CALCULATION PROCEDURE To obtain representative gas and liquid stream samples and to provide a quantitative measure of overall system Performance for comDarative purpLses, a thorough test of the field and plant system was conducted in the summer of 1957. Oil production at each battery was sta-

By T. E. Scott, D. H. Sherman, C. V. Owen

Mechanical properties and optical metallographic characteristics of vanadium containing 53 ppm (wt) H were investigated from, 77° to 298°K. A sharp ductile to brittle transition induced by the presence of hydrogen was observed between 238° and 223°K and a mar-tensitically formed hydride appeared at 200°K. While there appears to be a subtle relationship between the hydride formation and the ductile-brittle transition, it was concluded that the hydride per se was not sufficietzt to cause the severe em brittletnent. On the basis of the metallographic experiments and the results of a Petch analysis it is suggested that the mechanism of the embrittlement involves a reduction of the true surface energy, or cohesion, of the uanadiunz. THAT hydrogen can severely embrittle vanadium is well-documented;'-5 however, the mechanism by which hydrogen induces the observed embrittlement has not been established. It is not known whether the embrittlement of vanadium is caused by the formation of vanadium hydride or by a more subtle role of hydrogen. Until very recently6>' the solid solubility of hydrogen in vanadium at temperatures in the,range of the embrittlement was not known to a useful accuracy. In general, a severe embrittlement of the type produced by the presence of hydrogen in vanadium can be caused by changes in either of two properties of a metal. Either the yield stress of the metal is raised to the extent that plastic deformation at the tip of a crack cannot occur or the cohesive properties of the metal are reduced, at least locally, to the point at which cleavage is the natural response to applied loads. Of course a combination of these is possible. It is not known which of these properties of vanadium is influenced most by the addition of hydrogen. The purpose of this investigation was to determine the role of hydrogen in the embrittlement of vanadium. Accordingly, the solubility of hydrogen in vanadium in the temperature range where embrittlement is most severe was determined, the appearance of vanadium hydride was examined in relation to the initial ductile to brittle transition temperature, and an attempt was made to evaluate the effect of hydrogen on the yield stress and cohesive properties of vanadium. MATERIAL AND PROCEDURES Sample Preparation. The vanadium used in this investigation was prepared by the iodide refining process described by Carlson and owen.' Three ingots, 3 in. diam by 6 in. long, were cold-swaged to 0.096 in. diam, cut into short lengths, and then arc-melted under purified argon into one ingot. This process was repeated to insure a uniform composition in the final ingot. Chemical analysis of the metal is given in Table I. On the basis of work of Loria et a/ .' the following sequence of treatments was performed in order to obtain a uniform equiaxed ultimate grain structure: a) cold swage q-in.-diam ingot to 0.230 in. diam; b) anneal 6 hr at 1000°C in vacuum; c) by cold swaging reduce 81 pct in area in three steps: 0.230 to 0.187 in. diam, 0.187 to 0.150 in. diam, 0.150 to 0.096 in. diam. This sequence provided the desired grain structure after subsequent annealing treatments. Because annealing in evacuated quartz capsules resulted in contamination by oxygen, all anneals in this investigation were performed in a 304 stainless-steel chamber under a dynamic vacuum of 10- I Torr with the vanadium wrapped in tantalum foil. Prior to all annealing treatments the wires were electropolished for 1 min at 16°C in an 80 pct methanol-20 pct sul-furic acid electrolyte at 12.5 v. Following the final reduction the 0.096-in.-diam wire was cut into 2-in. lengths. A 1-in. gage section was reduced to 0.090 in. diam by electropolishing as above. Five different grain sizes were obtained by annealing the 2-in. samples at different temperatures for 8 hr to insure uniform grain size and residual hydrogen removal. The annealing temperatures used and the resulting grain sizes are given in Table 11. The final step in sample preparation was to charge half of the specimens of each grain size with hydro-

Jan 1, 1969

By H. T. Sumsion, A. U. Seybolt

The results of an investigation of vanadium-rich V-O solid solutions are presented, indicating the structure and lattice parameters of two solutions, a and ß, and their approximate temperature-composition existence. The a solution is the terminal body-centered cubic one, and contains up to 3.2 atomic pct 0. The ß solution has an ordered body-centered tetragonal structure, is formed at 1270°C, and exists from about 15 to 22 atomic pct 0. From the evidence available, the various phase boundaries have no appreciable temperature dependence. Evidence has been found for a polymorphic transformation in pure vanadium at 1550°C. IN an earlier investigation' dealing with the preparation of pure vanadium by calcium reduction of the oxide, it was found that small amounts of oxygen drastically reduced the ductility of the metal. Because this effect was so marked, it was decided to make a study of the solubility of oxygen in solid vanadium. This report deals principally with this solubility and the nature of the phase relationships in the vanadium-rich region, particularly at temperatures below 1300 °C. However, during the investigation enough data on the V-0 system were obtained to make it appear worthwhile to present a tentative phase diagram up to the composition VO. The only significant prior work found on this system are the contributions of Klemm and Grimm,' and Mathewson et al.3 Klemm and Grimm prepared a wide range of V-O compositions by powder techniques including the compositions VO.l, VO.2, VO.3 and VO4 (9.1, 16.8, 23, and 28.6 atomic pct 0, respectively). The first three compositions were found to consist of a body-centered tetragonal solid solution, while the last also showed lines of VO (NaCl structure). They found that the parameter c, increased and the parameter a, decreased with increasing concentration of oxygen. For their composition VO.27, or about 16.8 atomic pct O, they cite the values a, = 2.948A, c, = 3.53A, and c/a = 1.2. Klemm and Grimm made no attempt to determine the solid solubility limit nor to construct a phase diagram. They did, however, give some data on the homogeneity range of VO, and they proposed a structure for the body-centered tetragonal solid solution; these points will be taken up later. Materials and Preparation of Samples The vanadium used in this investigation was prepared in the laboratory by the method previously mentioned.' A typical analysis is as follows: Fe, 0.007 pct; Si, 0.02; Ca, 0.06; C, 0.224; O2, 0.044; N,, 0.0017; H2, 0.003; and V, 99.34 ±0.3 (assay). The vanadium assay is probably low by about the error given. The impurities total about 0.36 which, if subtracted from 100, gives a purity of about 99.6. At the time material was being prepared for this work no suitable technique was available for melting vanadium without appreciable contamination. The procedure adopted therefore was to cut the calcium-reduced regulii into slices which were then rolled to strip about 0.025 in. thick for oxygen diffusion. Pieces of rolled vanadium of approximately 0.025xY4xl in. and weighing about 0.3 g were suspended in a vertical fused-silica tube which was part of an ordinary gas absorption apparatus. The silica tube was heated by an electric resistance-tube furnace which could be raised around the silica tube or lowered away from it as desired. This apparatus had no novel features which require detailed description. Other than the silica tube and furnace, it consisted of a glass system evacuated by a liquid nitrogen trapped mercury diffusion pump, a mercury-operated gas burette, a McLeod and a Pirani gage, and a mercury manometer. It was also equipped with suitably located stopcocks for isolating various parts of the system; the vacuum ordinarily attained was between 10" and 10-6 mm of mercury. Oxygen generated by decomposing MnO2 was passed through anhydrous magnesium perchlo-rate before introducing it into the gas burette and thence to the absorption chamber.

Jan 1, 1954

IN comparing the living conditions of the worker or peasant of the past with those existing today, his-torians might point out many strange contrasts. From the Doomsday Book we learn that at the time of Wil-liam the Conqueror the 1,375,000 inhabitants of Eng-land and Wales owned less than 1000 horses and 5000 oxen. Even as recently as 1871 when England and Wales had a population of 31,845.000, the total number of horses in the country was estimated at 1,110,000. Compare the necessary drudgery of labor in those days with conditions in Canada today where a population of less than ten million people own 3,500,000 horses. Re-member that there is also a turbine installation in` this country of more than four million horse-power, besides steam boilers and locomotive and automobile engines which reduce the traction and hand labor of the farm and factory. Frequently, poetic license has glossed over the poverty and hardship of the common people in the "good old days," and the imagination has created an idyllic world, far from being justified by the condi-tions which actually prevailed. Simon Patten's de-scription of the Middle Ages as "A Thousand Years Without an Ice Box" came nearer portraying the true situation. No one is likely to forget that the discovery of America was an incident in Europe's attempt to find a short route to the Indies, but the fact is usually for-gotten that the summer diet in Europe in 1400-an ice-less age-was such that spices were more precious than gold. Though the glamor of the Indies may never sur-round the modern refrigerator, certainly the modern housewife is likely 'to feel that the applied art called "cookery? may attain to higher levels with the assist-ance-6f such an adjunct. Those who have spoken slightingly of the uniformity of the modern apartment and have eulogized some of the exceptional hand-made furniture which has been bequeathed by former generations, have failed to com-pare modern house furnishings with those in the typical peasant's hovel. Machine-made furniture, though with-out particularly good lines, contrasts quite favorably with the pile of rags in the corner, and the poorest gas or oil stove is better than an open fire on a dirt floor. The scientist's application of the theories of physics, chemistry, biology and mathematics .to practical prob-lems has brought about a series of kaleidoscopic trans-formations in agriculture, industry and commerce. Large scale production, improved means of communica-tion and the prevailing higher standard of living are terms which imply a very human meaning when in-terpreted as actual changes in individual living. Though the student and the teacher may deprecate the influence of commercialism upon science, humanity as a whole has received great benefits from the close relationship which has developed between science and industry, and industry in turn has done much for science through the building and endowment of laboratories and by supply-ing funds to maintain research workers.

Jan 11, 1927

By P. G. Shewmon, H. E. Collins

A study has been made to determine the sites at which sulfur adsorption occurs on copper surfaces. measurements were made of the relative torques, Ys, at the intersection of twin boundaries with surfaces near the three low-index orientations, i.e., (100), @lo), and 011), over a range of H2S/H2 ratios. HZS concerztvations j'ro~n 3 to 1500pp)n between 830" and 1050°C were used. It is concluded that sulfur adsorption occurved preferentially though not exclusively at edge sites near the (100) and (110) surfaces in the HzS range — 700 Ppm giving rise to negative torques near these orientations. Beyond this HzS range, adsorption occurred at all sites. Near the (111) surface, 7/y little with HzS concentration up to approxiwzately 75pptn. Above this range, the results indicate adsorption is occurring OH both terrace and edge sites. SCIENTIFIC interest in surfaces and their interactions with a gaseous environment dates back to the beginning of the 19th century. The scientific luminaries of that period—Faraday, Maxwell, Rayleigh, Dewar, and Gibbs—were already concerned about such processes. However, it has only been within the past several decades that adsorption on metal surfaces has been actively studied. This increased interest in adsorption has been brought about by the advent of new and improved experimental techniques and apparatus, e.g., ultrahigh vacuum, and field-emission and ion microscopes. However, most of the work done using these techniques has been carried out at low temperatures. When adsorption studies have been made at either low or high temperatures, they usually gave no indication of the particular surface orientations or type of sites on which adsorption was occurring. In the last few years, there have been a series of studies in which the surface tension, y,, and/or its derivative with respect to orientation, 7, have been studied as a function of orientation and atmosphere.'-7 Nearly all of the work on the relative torque,* ~/y, silver annealed in hydrogen and air.6 Recently Winterbottom and Gjostein" have used a modified and more accurate Mykurian method to determine the y plot of gold in hydrogen The only work in which T/~, has been measured over a range of chemical potentials for a given solute, p2, is that of Robertson and shewmon7 on the Cu-0 system. They measured T/Y, vs Po, (10"" to 10- l3 atm) at 1000°C in various mixtures of Hz0 and HZ. From this work they estimated the value of p2 at which one half of the surface sites are occupied with oxygen, pg, as being in the range 10- l6 to 10- l5 atm of oxygen. They also found that increasing Pa increased the magnitude of ~/y, near the (111) and (100) orientations. This indicates that oxygen is not adsorbed preferentially at step edges, but uniformly over all surface sites. In addition, they did one experiment on sulfur adsorption on copper surfaces, which indicated that sulfur adsorption decreases ~/y, near the (100) orientation, while not affecting ~/y, near the (111). This could be interpreted as indicating that sulfur adsorbs preferentially at step edges near the (100). In this paper the primary objective of the work has been to carry out a study of sulfur adsorption on copper surfaces over a range of temperatures and p,. In conjunction with this work, thermal grooving at grain boundaries has been examined as a method of determining the effect of sulfur adsorption on y,. METHODS Ideally, one would like to have information on the quantity of solute adsorbed on a surface and the types of sites at which it is absorbed as a function of p2. The total quantity adsorbed or the surface excess is given by the thermodynamic equation Thus data on the variation of y, with pz indicates the value of p2 at which adsorption becomes appreciable and the quantity adsorbed. The type of adsorption site is more difficult to deduce but information on this can be obtained from the variation of rz with 8, the angular deviation of the surface orientation. This is obtained from the thermodynamic equationlg Data on t and ys as functions of p2 have been obtained by the following methods. 1) Twin Boundary Grooving—By determining the effect of adsorption on the torque, 7, where T is the variation of surface energy, y,, with orientation, it is possible to obtain some indication as to the preferred sites of adsorption. Experimentally, the torque value measured is the relative torque, 7/ys The twin boundary grooving technique suggested by Mykura'' was used in this study to determine near the three low-index orientations— (loo), (110), and (111). Mykura's equation relates 7 /yS to measurements of the di-

Jan 1, 1967

By L. Stone, H. Margolin

The Ti-C-N and Ti-C-O systems were investigated in the temperature range from 500° to 1400°C and in the composition range up to 2 pct C and 5 pct N or 0. Characteristic isothermal sections at 800°, 900°, 1000°, and 1300°C are presented. The Ti-N-0 system was studied in the temperature range from 900' to 1400°C with alloys containing up to 6 pct total alloying content. Characteristic isothermal sections at 1000° and 140O°C are presented. Melting-point data for all three systems are also included. THIS paper reports on one of a series of investi-gations which have been conducted on the phase diagrams resulting from interstitial alloying with iodide titanium. The other investigations involved delineation of the binary systems with carbon,' nitrogen and boron,h and oxygen. The Ti-0 binary system has also been investigated by Bumps et al.' In varying degrees, each of these interstitial elements has been shown to stabilize the low temperature a modification of titanium1-5 and each forms a face-centered cubic TiX compound (henceforth designated 6). In addition, the Ti-N and Ti-0 systems reveal a low temperature tetragonal phase (6) formed by a peritectoid reaction between a and TiX Experimental Procedure The development of experimental techniques for the study of titanium alloy systems has, to a large extent, become standardized. In this investigation, the equipment and procedures described in detail by Cadoff and Nielsenl have been used. Arc Melting: In general, binary alloys with carbon, nitrogen, and oxygen, prepared in the composition range of interest in this investigation, show negligible composition changes during arc melting. However, the possibility of the formation of some gaseous combination of alloying elements such as CO, CN, or NO during the preparation of these ternary alloys was considered. Calculations showed that the evolution of only 0.05 gram of such a gas would be detectable as a pressure change in the closed system used during preparation of these alloys. Such pressure changes were not observed. Consequently, nominal compositions have been used in plotting the data. The compositions of the materials used in the preparation of the alloys are shown in Table I. After melting for 3 to 5 min at 275 to 350 amp, the alloys were checked for homogeneity by microstruc-tural examination. Alloys containing up to 1 pct C were homogeneous in the presence of less than 3 pct N or 0. At higher alloying contents, some inhomo-geneities in the carbon distribution became evident. Alteration of the melting procedure toward longer times and higher currents did not improve the homogeneity of these alloys. Ti-N-0 alloys were homogeneous in the range to about 3 or 4 pct total alloying addition. Beyond this, almost all of the specimens showed as-cast microstructures consisting only of the phase. Consequently, inhomogene-ities could not be detected by examination of micro-structures. Ten alloys from each of the systems were analyzed for two of the elements present (oxygen being omitted in all cases and titanium being omitted in the Ti-C-N alloys). In all cases the analyses were found not to be sufficiently precise to serve as criteria for the total composition of these alloys. On the basis of phase distribution in heat-treated alloys, however, it appears that carbon is distributed throughout the alloys most uniformly, with oxygen and nitrogen following in that order. Heat Treatment: Specimens for heat treatment were wrapped in titanium sheet before sealing in the argon-filled quartz capsules. Heat-treatment times varied from 100 hr at 800°C to 0.5 hr at 1400 °C. After heat treatment the specimens were quenched by breaking the capsule in water. With the exception of alloys in the low composition region, heat treatment did not have an appreciable effect on the as-cast microstructures. Metallography: Following heat treatment, the specimens were prepared for metallographic examination by grinding on emery paper and electrolytic polishing. For the majority of the specimens a 10-sec etch with Remington "A" agent (25 pct HNO3, 25 pct Hf, and 50 pct glycerin) adequately

Jan 1, 1954