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By B. I. Routh

A STUDY of the effects of temperature on the gel strength of drilling muds is a natural outgrowth of the present era of deep drilling. The control of the gel solids' is now considered important because it affects the wall-building qualities; the suspension of weighting material; the removal and release of sand, cuttings, and gas; and the control of cav-ing formations. With regard to the effect of temperature on gel strengths Herrick2 states: "Temperature variation within ordinary limits does not have much effect on yield points." Lewis, Squires and Thompson3 investi-gated one clay and found no marked change with temperature in either yield point or mobility. Reed4 found that potassium bentonite showed a great increase of gelation with increase in temperature and qualitatively there occurred a marked increase in viscosity upon heating. The apparatus used in these experiments consisted of a Stormer viscosimeter, Marsh funnel viscosimeter, rectangular and cylindrical shearometers, Mudwate hydrometer, and other minor laboratory equip-ment. The various methods of measuring viscosity and gel strength have been extensively described by Evans and Reid.5

Jan 1, 1938

By Stanley F. French, Bruno F. Koch

Although the amount of dust that will be actually recovered in the six main dust-control systems cannot be accurately stated until the tests mentioned previously are carried out, it is estimated that the average air entering the wet collectors will contain around 5 grains of dust particles per cubic foot. This means that the six systems handling a total of about 133,000 cu.ft. of air per minute will return about 68 1/2 tons of dust to the concentrator per day and since the copper in this dust will average around 2 per cent, the total recovery is approximately 1.37 tons of copper every 24 hours. This important copper recovery is not due entirely to the dust-control system since in a plant without control only the duct that is dispersed to the atmosphere represents a loss. A conservative estimate of the recovery of copper solely due to the dust control system would be about half of the total or approximately 0.70 tons of copper per day.

Jan 1, 1942

By M. D. Everell

A study has been made of the relationships between grinding selection functions and physical properties of rocks, particularly the failure loads of irregular particles and the compressive and tensile strengths of large regular specimens. The rocks used were limestones of various structures and impurity contents, a carbonatite, and a high-purity crystallized calcite. The selection functions were obtained from carefully performed grinding experiments on selected narrow size ranges in various grinding machines-a laboratory batch ball mill, a Hard grove grindability machine, and a mill of the type suggested by Yang, Mempel, and Fuerstenau. The specific rates of breakage during milling and the failure loads of irregular specimens correlated well for the rocks studied. The testing of irregular particles is suggested as a means of predicting the behavior of commercial mills.

Jan 1, 1973

By HOMER L. WILLIAMS

WHILE some of the mining companies have been pumping a small amount of water for some time, it is only in recent years that large quantities of water have been encountered in the Tonopah district. The water appears to be in different zones or belts so that the draining of one property does not necessarily affect the one adjoining. Consequently, each company has its own pumping plant and its own conditions. The companies panes handling the largest amount of water are the Tonopah Extension Mining Co., Halifax Tonopah Mining Co., West Tonopah Consolidated Mining Co., and Great Western Consolidated Mining Co. The Halifax shaft is on the eastern end of the district and the other three properties on the western. The ore-bearing formation occurs at greater depth on -the eastern and western ends, hence the water problem in these properties.

Jan 1, 1921

By Eizo Yabuuchi, Yukito Imanaga

INTRODUCTION In treatment of mine drainage, it is well known that the neutralization by calcium carbonate is far better than by slaked lime because of cheaper cost and better precipitability of its deposit. However, in case of iron ion contained in the mine drainage consists of ferrous salt, the ferrous salt must be oxidized to ferric salt before neutralization, because the ferrous salt does not react with calcium carbonate. At Yanahara Mine, during the period of 1950 through 1956, ferrous ion in the mine drainage had been oxidized to ferric ion, simultaneously neutralized by adding calcium carbonate into the aerated drainage. During the period of 1961 through 1974, after passing through many kinds of treating methods, the neutralization had been carried out by addition of calcium carbonate into the drainage after oxidized its ferrous ion to ferric by using nitrous gas as an oxidizing catalyzer. Meanwhile we had made an experiment on the oxidation of ferrous ion by utilizing iron bacteria, and developed a method which oxidized ferrous ion in large quantities briefly by cultivating and concentrating iron-oxidizing bacteria. Since 1974, we have been operating successfully for treating the drainage at Yanahara Mine by means of utilizing these bacteria.

Jan 1, 1976

By Robert G. Van Nostrand, John H. Henkel

TRANSIENT potentials obtained in resistivity prospecting can be separated into two classes. The first is electromagnetic, has a comparatively short time constant, and increases in relative amplitude as the electrode separation is increased. These electromagnetic transient potentials, of which an excellent theoretical treatment is given by Yost: are the result of changes in the current and can be classed as differentiated signals. The second class is electrochemical, has a comparatively long time constant, and decreases in relative amplitude as the electrode separation is increased. The electrochemical signals are generated by the current flow itself and can be classed as integrated signals. The transient potentials due to electrochemical factors are the subject of this article. The phenomenon is referred to as induced polarization. Schlumberger" was the first worker to observe induced polarization, but he was unsuccessful in attempts to apply the principles of induced polarization in electrochemical prospecting. Other workers, notably Bleil; have studied polarization and in some cases pointed out its possibilities, but no theory has been presented that describes polarization and its time dependence adequately. It is the purpose of this discussion to present the essence of a theory to geo-physicists and to show that it leads to results consistent with experimental evidence. The theory on which this analysis is based has existed in electrochemical circles since 1910."

Jan 1, 1958

By A. B., Sabin

THERE are many who know The Lucky Tiger and will remember the 35-mile road from Esqueda, a station on The Nacozari Railroad in northern Sonora, Mexico. They will remember the box canyons of the Agua Caliente Mountains which are scarcely wide enough for two cars to pass; the Bavispe River which one hour may be a lazy trickle and the next a sweeping torrent, and the tortuous road up Tigre and Espuela canyons, now following the wash, now hugging some gigantic red cliff. It is still the same. From camp the view of the distant blue-gray mountains is the same. But one thing a visitor of a former day might miss: The hundreds of pack mules and burros, loaded with concentrates from the mill, which used to take most of the road and show up at the most inopportune places, have almost disappeared, replaced of course by the auto truck.

Jan 1, 1929

By M. L. Brashears

IN the last 15 years industrial use of ground water has more than doubled, and in 1951 amounted to 5 billion gallons per day. A similar sharp increase in the utilization of ground water for irrigation and public-water supply occurred in the same period. In many areas rapid increase in withdrawal from wells has taken place almost entirely unhampered by regulatory control and with little or no integration of effort. As might be expected, the chief interest in many regions has been maximum production rather than sustained perennial yield. As a result, widespread depletion of underground reservoirs and deterioration of the quality of the water stored in them has taken place in many areas, even though total pumpage in the United States is far below ultimate potential. Of even more concern is the fact that excessive withdrawal has drawn salt water into the reservoirs beneath many heavily populated centers along the Atlantic, Gulf, and Pacific coasts, causing costly abandonment of pumping plants.' Many hydrologists expect that consumption of water will rise rapidly in the near future, and some predict that industrial requirements will more than double in the next decade.2,3 Thus it appears likely that the draft on many already heavily pumped underground reservoirs will be greatly increased and the search for additional sources of usable ground water intensified in years to come. In view of this, industry as a whole will be forced more and more to recognize the potentialities and limitations of ground-water reservoirs and to utilize them more effectively to prevent costly water shortages and disruption of production. Through painful experience, some industries are already well aware of the need for effective water utilization, and have managed individually or through joint effort to check trends threatening to deplete underground reservoirs completely or to impair the quality of the water. Various remedial measures have been used to bring about successful management of local or regional ground-water resources. Of these, replen-ishment of aquifers by recharge wells or basins has played an important role in overcoming some ground water problems. Artificial recharge of underground reservoirs by water spreading has been practiced successfully in the United States for many years. In the West it has become an important method of salvaging flood run-off for irrigation of crops and maintenance of public water-supply reserves, and it is used to some extent in parts of the East. Artificial recharge by means of wells, on the other hand, is a relatively new development. Until recently it was employed in only a few areas, principally along the East coast. For the last few years, in the ever increasing search for additional water supplies, industry has had greater recourse to this method. Utilization of recharge wells to control the temperature and quality of underground water supplies is also being considered seriously. Operation of recharge wells, like water spreading, is governed largely by local conditions. It requires water relatively low in turbidity, whereas in some areas water spreading has been used successfully with water of high turbidity and silt content. However, water spreading must be employed in large areas and can be carried on effectively only where aquifers crop out at the surface. Recharge wells can be used in limited space. Recharge wells are similar to production wells except that the water flows in the opposite direction. Thus any water-bearing bed that will yield water to wells may be recharged by wells. Often, however, the water available for recharge is of a different character and temperature from that existing in the ground-water reservoir and if transmitted directly underground from a recharge well to a production well might require expensive or difficult treatment before it could be used. Fortunately the physical characteristics of reservoir beds, which control the movement and behavior of ground water, are generally not homogeneous. Moreover, the movement of ground water is very slow because of the frictional resistance of the reservoir beds. By taking full advantage of hydrologic and geologic conditions, it is therefore possible in many instances to bring about favorable changes of temperature and dilution as the water moves from the recharge wells underground to the production wells. Furthermore, if the natural quality or temperature of ground water is unfavorable for industrial purposes, recharge wells may be used to introduce water of more favorable quality or temperature into the ground-water reservoir. When water is discharged into a recharge well, the head in the well is increased. Because of this, a cone of elevation is produced on the water table or the artesian pressure surface in the area surrounding the well. The cone of elevation is similar to the cone of depression produced around a pumping well except that the apex of the cone is above the water table or artesian pressure surface. Thus if a recharge well and a production well tapping the same water-bearing bed are close together, as would be the case at many industrial plants, some of the water discharged from the recharge well would be drawn into the production well within a short time. Under such conditions it is apparent that water of unfavorable temperature and chemical characteristics should not be used for recharging. The more important ground-water reservoirs in the United States often consist of alternating layers of impermeable beds and porous material that will yield water readily to wells. Physical characteristics of individual beds in a ground-water reservoir may not persist over great distances, the impermeable layers grading into beds that will yield large quantities of water. Thus the water-yielding material in underground reservoirs, whether large or small,

Jan 1, 1954

By Prakash C. Kapur

Many balling and gradation system6 generate self- similar size distributions of the agglomerates. Inspection of the experimental data shows that this is also true of the steady state distributions resulting from the granulation of coarse, partially wet powders, for example, the fertilizer feeds. This result is exploited in the derivations of a number of simple and useful relationships that are pertinent to the analysis of these agglomeration systems. The bonding liquid demand of the granulating charge is a third order polynomial function of the dimensionless ratio of feed particle size to median granule diameter in the weight-fraction distribution. The median size, in turn, is the scale factor or characteristic size parameter in the similarity distribution. The granule size distribution, therefore, is completely specified by the liquid content and the similarity function, and so are the process efficiency and the ungranulated component In the product at steady state.

Jan 1, 1977

By AIME AIME

MINERAL production of the United States is valued at over five billion dollars a year at present and the industry employs close to a million workmen, yet such maps as are available that might indicate the geographical distribution of this industry show only the location of coal and oil fields and of other mineral deposits. No recent map is available that shows this distribution in a quantitative way. The purpose of the maps and graphs here presented is twofold: (1) to give the mining engineer a clear conception of the relative value and the pattern of distribution of minerals in the United States; (2) to test the so-called block-pile (or grouped pillar) system of statistical mapping, which makes this presentation possible. (I discussed this method of mapping in an article which appeared in Economic Geology in 1939, Vol. 15, p. 185-188.)

Jan 1, 1941

"Mining as an industry of Utah had its inception in the activities of United States soldiers who came to the Salt Lake valley under the command of Gen. P. E. Connor, founder of Fort Douglas, in October, 1862. Many of these soldiers were from California and naturally employed their spare time in the search for minerals. Although their military status did not permit them to make locations in their own names, they assiduously prospected the region in accordance with their own knowledge and with information conveyed to them by Indians and others. Their efforts were encouraged by their commander, who thereby fairly earned the title of father of the industry here, and by their other officers, and many discoveries that subsequently proved of great value were made by the soldiers.No systematic prospecting or mining had been done in the Territory previously, although early Mormon settlers in the southern portion had mined a little ore from time to time in order to provide supplies of lead for bullets. The Mormon leaders at that time did not encourage mining. They held that agriculture was more important and profitable for their followers.Coal was discovered and produced in 1850. Iron was discovered in 1850 and the first iron plant was in operation in 1852 in Iron County. The first non-ferrous metal production was in 1854, in Beaver County, when Isaac Grundy treated ore from the Rollins mine in what is said to have been the first lead furnace west of the Rocky Mountains. The first mineral location was the West Jordan claim in Bingham canyon, located September 17, 1863, now owned by the United States Smelting, Refining & Mining Co., and still productive. The first district organized in the state was the West Mountain (Bingham), December I 7, 1863. Other important districts of early organization are: Little Cottonwood, December 20, 1869; Big Cottonwood, July 11, 1870; American Fork, July 21, 1870; Uintah (Park City), July 8, 1871; Tintic, December 13, 1896; Ophir, August 6, 1870. The first silver-lead smelting was by J. W. Gibson at Stockton in 1866. Lieut. James Finnerty had previously erected two small trial furnaces there, but made no quantity production."

Jan 1, 1925

Executive Committee. ROBERT H. RICHARDS, Chairman. ALBERT SAUVEUR, Vice-Chairman. TIMOTHY W. SPRAGUE. HENRY A. WENTWORTH. AUGUSTUS H. EUSTIS, Secretary, 131 State St.., Boston, Mass. The twelfth meeting of the Boston Section was held at the Engineers' Club, 2 Commonwealth Ave., Boston, on Monday evening, May 5, 1913, fifteen members and three guests being present.. The meeting Was called to order by Vice-Chairman Albert Sauveur, Who introduced the speaker of the evening, Utley Wedge, of Ardmore. Pa. Mr. Wedge read a, paper on the chloridizing roasting of copper ores, Which lie illustrated With a stereopticon, and Which will be published in full by the Institute. After Mr. Wedge had closed his paper, Which was received with great interest by all the members. the following discussion took place: Professor Hofman said that iron was formerly thought to bo essential to the Henderson process, but that it is not absolutely essential. Mr. Wedge said that., as far as he knew, the presence of some sulphates Was an absolute necessity, and that lime ores can be worked satisfactorily, although lime has an effect on the subsequent leaching. He added that the low fuel consumption of the latest Wedge furnace is a result of direct application of the combustion gases to the ore. Ten per cent. of fuel Was needed with the muffle furnace. By direct firing lie has been able to reduce the fuel needed to from 2 to 4 per cent. In the latest types of furnaces the uses from the upper hearth are not used. There is doubtless some tem-perature at Which the loss from copper chloride volatilization becomes serious, but in practice on Rio Tinto ores troublesome losses are not experienced.. The copper apparently does not become volatile at the temperatures where we would expect that it would. There are doubtless ores in which there would be serious danger from losses from this source. The latest furnaces do not use the high temperatures that Were needed in the former single-hearth Wedge furnaces.

Jan 7, 1913

By Alfred F. Beasley

The slags derived from the smelting of lead and copper ores are composed essentially of silicates. The problems arising from the smelting of these ores consequently involve the study of silicate fusions. In the absence of specific knowledge concerning the compounds occurring in slags, it has been the practice of metallurgists to treat them in terms of their total chemical composition. Slags have been classified as monosilicates, bisilicates, sesquisilicates, and subsilicates according to the relative amounts of oxygen in the acid and basic radicles of the hypothetical salt produced. While this has been a useful guide to metallurgists in computing the furnace charges, it falls far short of a basis for the scientific investigation of slags. In order to understand the nature of a slag as a whole it is necessary to learn the physical and chemical properties of the mineral compounds which go to make up that slag. The efficiency with which an ore is smelted in a furnace depends primarily on the physical properties of the compounds formed during the operation. When the melting points and fields of stability of each of the mineral compounds in slags have been established, it will be possible to determine the properties of any given slag by examining the nature and amounts of its mineral constituents. Earlier Investigations In 1884 and succeeding years an extensive survey of lead and copper furnace slags was made in Europe by Vogt, and a large part of the present knowledge of the subject is due to his publications.' Vogt's interest in artificial fusions was directed primarily towards the explanation of problems in igneous and economic geology and his subsequent works have been confined wholly to that subject.

Jan 1, 1930

Executive ARTHUR S DWIGHT, Chairman B THAYER CHARLES F RAND P MATHEWSON J V W REYNDERS Membership WILLIAM H BASSETT, Chairman W Y WESTERVELT Vice-chairman P MATHEWSON H G MOULTON F T RUBIDGE Finance WALTER H ALDRIDGE, Chairman GEORGE D BARRON GALEN H CLEVENGER

Jan 1, 1923

By N. S. Stoloff, R. C. Ku, R. G. Davies

The stress-strain behavior of Fe-Co and Fe- V alloys containing up to 25 pct solute have been studied in the temperature range 25° to - 196°C. The microyield stress is independent of temperature for all alloys studied, while the temperature dependence of the ordinary yield stress is large and comparable to that for unalloyed iron. An alloy-softening phenomenon is observed for many alloys relative to unalloyed iron, and appears to be a consequence of removal of inter-stitials from solution and their subsequent agglomeration. The ductile to brittle transition temperature is increased markedly by both cobalt and vanadium. Transmission electron microscopy observations reveal that cross slip and cell formation are restricted with increasing solute, which can account for many aspects of yielding and fracture behavior. IRON and other metals of bcc structure slip on many planes of the (111) zone at moderate and elevated temperatures, giving rise to wavy glide. At low temperatures, however, there is a tendency for slip to be restricted to planes of only one or two crystallographic types; in the case of Fe-Si alloys for example, (110) glide predominates, giving rise to planar slip bands."' Restriction of cross slip at low temperatures in iron has been linked by Brown and Ekvall3 to increased strain hardening in the preyield microstrain region, leading to an apparently large temperature dependence of the yield stress. Support for this view has been provided by Lawley and Gaigher4 from a transmission electron microscope study of molybdenum. They concluded that dislocations at lower temperatures, by virtue of their inability to change planes readily, are unable to interact and annihilate, leading to an increase in internal stress and work-hardening capacity. Restriction of cross slip at low temperatures has also been suggested to be an important factor in determining the ductile to brittle transition of single-phase solids, including metals of bcc structure.5 It is pertinent to note that most solute elements tend to raise the ductile to brittle transition temperature of poly crystalline ferrite,6,7 although in some cases, e.g., Fe-Cr7 and Fe-Al,8 the dilute alloys may actually yield at lower stresses than unalloyed iron. It appears, therefore, that solute elements may have an effect analogous to lowering the test temperature with regard to restricting cross glide. Such an effect has indeed been observed in the ionic alloy system KCl-KBr,9 in which bromine atoms, although causing little misfit and consequently little effect on the yield stress of KC1, have a pronounced effect in restricting wavy glide and inducing brittleness. The purpose of the present investigation was to determine the effects of selected solute atoms on the yield stress and fracture behavior of iron, and to elucidate in turn how the slip character was related to these properties. Since it is known that interstitial atoms exert a strong influence on the mechanical behavior of iron, the solute elements chosen for study were vanadium, which reacts strong with interstitials,10 and cobalt, which does not form highly stable interstitial compounds." EXPERIMENTAL PROCEDURE Four-pound ingots of each of the following alloys were vacuum-melted in zirconia crucibles: Fe-1, 5, 10, 25 at. pct Co, and Fe-1, 4, 10, 20 at. pct V. An ingot of unalloyed iron from the same original stock as that used for the alloy was remelted under similar conditions to eliminate variations in interstitial content arising from differing thermal histories. Chemical analyses of the iron, cobalt, and vanadium melt stock are listed in Table I. All ingots were rolled and swaged, commencing at 850°C, to 1/4-in.-diameter bar. The bars were then annealed at 850°C for 1 hr (except that the 10 and 20 pct V alloys were heated for 2 hr) to give a uniform equiaxed grain size of about 0.05 mm. Tensile samples of 0.125 in. diameter by 0.8 in. gage length were utilized for studies of the ductile to brittle transition. A second set of tensile samples were utilized for microstrain experiments in which strain sensitivity of 1 x 10"6 was achieved by a capacitance method.3 Cylindrical compression samples 0.250 in. diameter by 0.4 in. long also were prepared to study the influence of composition on the macroscopic yield stress, and for metallographic analyses of defor-

Jan 1, 1965

By H. W. Schadler

The superplastic behavior of low carbon and manganese bearing steels has been evaluated. The results of elevated-temperature stress-strain rate and elongation tests are reported which indicate that high strain rate sensitivity (>0.5) and adequate elongations are achievable in ultrafine-grained steels 1 to 2 p, but at strain rates which are not commercially attractive. It has been demonstrated that the fine grain size is retained after long times and high strains if the temperature is kept within the range of the two-phase (a + ?) field. INTEREST in superplasticity has been stimulated by the desire to: 1) understand the origin of, and mechanisms responsible for, the large uniform elongations observed, and 2) exploit this property for commercial advantage in metal forming operations. Although the Zn-22 wt pct Al alloy presently being studied as a model material1-5 may find application in sheet forming and extrusion, the potential of super-plasticity should best be realized in large tonnage materials, such as steel and aluminum alloys. The degree of superplasticity in low-carbon and manganese-bearing steels has been evaluated. The results of elevated-temperature stress-strain rate and elongation tests on ultrafine grain size material are reported. Avery and Backofen6 and Hart7 have shown that geometrically stable flow leading to extensive uniform elongation in the tension test is associated with high values of the strain rate sensitivity, m, defined: Lozinsky had reported that titanium and zirconium experience permanent deformation if subjected to a constant load and cyclic heating through the temperature range of the phase transformation. Although strain rate sensitivities in excess of about 0.2 had not been reported previously for steel, permanent deformation had been observed11-13 in a wide variety of steels subjected to a constant load and cyclic heating through the temperature range of the a-? phase transformation. Thus by analogy, steel could be expected to exhibit high strain rate sensitivity but only in the a + ? condition. High strain rate sensitivity has been observed at 650°C (a + Fe3C), but not reported as such, by Bailey, Dickenson, and pearson14 in 1931 at a strain rate of about 10-9 per min. It then remained to determine whether high tensile elongations would be observed in a rate-controlled test at constant temperature and at what strain rate strain rate sensitivity values greater than 0.5 would be observed. Since previous experience8 had indicated the importance of fine grain size to realizing high m at reasonable strain rates, it was first necessary to produce an ultrafine grain size and then keep the grains from growing during the test. The results of this investigation show that fine grain size can be readily produced16 and maintained by restricting the temperature of testing to below the ? transus. Further, superplasticity (high m and large uniform elongation) is observed. However, the strain rate range is only marginally useful for commercial forming operations with the finest grain size produced. MATERIAL The material investigated initially was a 1.9 wt pct Mn, 0.42 wt pct C, hot-rolled bar previously used by Low and Turka1015 and available in the laboratory. The 0.500-in. round was cold-rolled to a 0.090-in. flat, annealed for 4 hr at 850°C in argon, air-cooled, and cold-finished to 0.050 in. Subsequently, four additional steels of the compositions given in Table I were investigated to explore the effects of manganese, carbon, and test temperature on the observed stress-strain rate behavior. These steels were melted under argon, cast to 0.75 by 2 by 5 in. slabs, hot-rolled at 850°C, surface-finished to 0.13 in., and cold-finished to 0.050 in. Sheet tensile specimens 0.200 in. x thickness with 1- or 2-in. gage length were cut parallel to the rolling direction. Table I also includes the nominal transformation temperatures for the AISI 1340 and the four experimental steels. EXPERIMENTAL PROCEDURE Production of Fine Grain Size. Ultrafine grain size (1 to 5 p) was considered essential for this studv. Grange16 has described two techniques for producing

Jan 1, 1969

By Howard N. Eavenson

WASTE of coal, or perhaps more properly the percentage of its recovery in mining, has keenly interested me during an experience of over a half century in coal mining. In the early part of that time and until a few ears after World War I the use of better mining plans and supervision resulted in an increased recovery. Since then, and particularly since controlled prices have been effective and mechanized mining has been extensively practiced, the tendency has all been toward lesser recovery in mining. The purpose of this paper is not to criticize the methods being used, which after all are the result of economic forces, nor to point to any particular mining method or to any locality where the best recovery is obtained. but to call attention to the tremendous waste of our national coal resources that is constantly continuing. A possible method of reducing this loss will be suggested. but without any illusions that it will be followed or that much attention will be paid to it.

Jan 1, 1946

By E. T. Turkdogan, W. L. Worrell

The rate of reaction of hydrogen sulfide with ferrous sulfide was studied by measuring the initial rates of sulfidation of iron strips in hydrogen sulfide-hydrogen-argon mixtures at 670°, 800°, and 900" C. The time-dependent surface sulfur activity is derived from the instantaneous rate of sulfidation with the assumption that diffusion in the sulfide layer is in a pseudo-steady state with the gas-sulfide chemical reaction. The rate of sulfur transfer from hydrogen sulfide to the surface of iron sulfide is proportional to the partial pressure of hydrogen sulfide and inversely proportional to the activity of sulfur at the surface of the sulfide layer. The derived rate equation is based on the assumption that most of the surface sites on the chemisorbed layer of iron sulfide are occupied by sulfur atoms and that the slow rate-controlling reaction is the dissociation of hydrogen sulfide on the chemisorbed layer. The experimental results are in reasonable accord with this reaction model. 1 HE slow approach to parabolic growth rate in the sulfidation of iron in hydrogen sulfide-hydrogen mixtures is a manifestation of slow approach to surface equilibrium between the gas and the surface of the sulfide layer. For example, at 800°C and Fig. 7 in Part I, the parabolic growth rate begins after approximately 1 day of sulfidation time. With decreasing temperature and decreasing partial pressure of hydrogen sulfide, the time necessary to reach gas-sulfide surface equilibrium is much longer. These observations are similar to those reported previously by Turkdogan et al.' on the oxidation of iron to wustite in hydrogen-water vapor mixtures. The slow approach to gas-sulfide equilibrium is well-demonstrated by the results in Fig. 1 where the square of the weight gain per unit area, ( g S per sq cmI2, is plotted against time for gas mixtures having PH g//>H = 1.0 with 0, 25, 50, and 67 pct Ar at 800°C. The value of 1.5 X lo-' (g S per sq cm)' corresponds to almost complete sulfidation of the iron strip (- 0.05 cm thick) to iron sulfide. The points fall on S-shaped curves. If the inflection parts of the curves are considered to be linear, thus indicating parabolic growth rate and the establishment of gas-sulfide equilibrium, their slopes would have to be the same for a fixed ratio in the gas mixture. Such is not the case, and the slopes for the "linear" parts of the S-shaped curves are lower than the value when gas-sulfide surface equilibrium is established. The subject matter of this paper is the kinetics of the surface reaction of hydrogen sulfide with iron sulfide during the early stages of sulfidation of an iron strip. EXPERIMENTAL RESULTS The apparatus and materials used were the same as those discussed in Part I. In the present experiments of relatively short duration, a purified iron strip, 5 by 2 by 0.05 cm, which was suspended in the uniform hot zone of a vertical zircon tube, reacted with a flowing gas mixture of hydrogen sulfide-hydrogen-argon. The sample was suspended from a gold chain attached to a calibrated silica spring. The amount of sulfur picked up by the iron, which formed a layer of iron sulfide, was determined by measuring the displacement of a reference point on the silica spring, using a cathetom-eter. In all cases, the degreased sample was first annealed in a stream of oxygen-free dry hydrogen for several hours to remove any impurities such as oxygen, nitrogen, or carbon which might have been present on the surface of the sample.' The rate measurements were carried out at 670°, 800°, and 900° C in hydrogen sulfide-hydrogen-argon mixtures with pH2 s/Ph2 ratios from 4 to 0.1. In a few experiments of short duration no sulfur deposition was observed in gas mixtures with (comments concerning sulfur deposition at high pH s/ph ratios were made in Part I.) Typical examples of the results obtained are shown in Fig. 2 for two temperatures and two gas compositions. With the present experimental technique, reproducible rate data could be obtained only after a uniform

Jan 1, 1969

By NEWTON B. KNOX

PERU, lying south of Ecuador and having common frontiers with Brazil, Chile, and Bolivia, includes over a thousand miles of the Andean mountains. The coastal plain is arid and narrow and the Amazonian jungle region is of interest only on account of its oil and gold placer possibilities. The mountain zone, however, here forms one of the world's most highly mineralized regions. The Peruvian Andes, like their Bolivian and Ecuadorian counterparts, form two distinct chains separated by the great Apurimac and Maralion valleys; but these rivers cut through the Eastern range to join the Amazon drainage, and the central valley is missing north of the passes thus formed by these rivers; the localities where the ranges are joined are aptly called knots. In addition, in central Peru, there exists a third range lying to the east of the first two and separated from them by the Urubamba and Huallaga Rivers. The Eastern range, however, is of little importance to the miner for few metal deposits are to be found therein except for the gold mineralization in the South. In general, deposition of metals in the Peruvian Andes accompanied igneous intrusions which invaded the folded Paleozoic and Mesozoic rocks during the Tertiary; thus the ore bodies are all typical of shallow or moderate depths.

Jan 1, 1945

By J. W. Sandelin, L. S. Birks

The group five metals, vanadium, niobium, and tantalum all show cold-rolled textures of {100)(011) and {112)(0ll) with a preference for the (100) in vanadium and niobium and for the {112) in tantalum. Recrys-tallization texture of (100) and (111) was reported1 for vanadium after annealing (no temperature stated). For tantal~m ,~ annealing below 1200°C strengthened the (112) texture but the (111) texture increased and was predominant as the annealing temperature was raised to 2500°C. Annealing niobium up to 1100°C strengthened the ( 100) texture and developed a weak (111) texture.' In the present work niobium has been annealed up to 2000°C. Nearly 70 pct of the grains showed {111) texture with only a weak (112) component and an insignificant (100) component remaining. In addition, double-crystal rocking curves were used to follow the increase in crystal perfection of the grains with increased annealing time. Material and Treatment. Samples i by 4 in. were sawed from & -in.-thick cold-rolled niobium sheet obtained from Wah Chang. Chemical analysis of the material showed it to be 99.4 pct pure with tantalum as the major impurity. Individual pieces were annealed for 2, 15, 30, and 60 rnin in a vacuum of 10'* Torr using an rf generator. They were etched until the grain boundaries were well-defined, Fig. 1. Average grain size varied from 1 mm for 2 min annealing to 2 mm for 60 rnin annealing. Experimental Results. Preferred Orientation. The orientations of 97 of the 117 grains in the specimens of Fig. 1 were determined by back-reflect ion Laue patterns. A General Electric 10-cm-diam cylindrical camera was used rather than the conventional flat camera in order to record more of the low-index spots. The method proposed by Forest, Barton, and schieltz4 was used to transform the cylindrical film patterns to standard stereographic projections. Table I gives the compilation of data. Even 2 rnin anneal at 2000°C is sufficient to yield a strong (111) preferred orientation, and the percentage of grains with this orientation increases steadily with annealing time at the expense of all other orientations. Crystal Perfection. X-ray topographs were taken of each specimen in both the (111) and (112) orientation using the method described by Birks and Grant.' As the anneal time increases, the grains become larger and the individual reflections become slightly more uniform in intensity, indicating an increase in crystal perfection. For a more quantitative measure of crystal perfection, it was necessary to measure the double-crystal rocking curve. The spectrometer employed was a Gaertner instrument of Compton design. LiF was chosen for the first crystal because the (400) reflection with d spacing of 1.05 AU is a good match to the (222) niobium reflection with d spacing of 0.95 AU. CuKp radiation was used in order to further reduce the d spacing mixmatch correction.' A variable aperture was placed between the LiF and the niobium specimen so that a single grain or even a small portion of a grain could be examined. Fig. 2 shows typical rocking curves for the four annealing times. For the 2-min specimen, a single peak is observed with 10' of arc full-breadth at half maximum. As the annealing time is increased to 15 or 30 min, several sharper peaks of 40 to 80" breadth can be seen within a single grain. After 60 rnin anneal only a single peak of about 30" is observed. Table I1 shows the corrected rocking curve breadths and the dislocation densities, ND. The latter were calculated from the equation7 where W is the corrected rocking curve breadth at half maximum in radians and b is the effective Burger's vector. For (110)(111) slip in niobium, b is 2.86 AU. Discussion. The annealing of cold-rolled niobium at 2000°C causes rapid preferential growth of grains with {ill} orientation. After only 2 rnin annealing time, 35 pct of the grains have the (111) orientation, and after

Jan 1, 1968