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The official Institute reports for the year 1929 were distributed in pamphlet form at the Annual Meeting, February, 1930, and were later included in Section 2 of Mining and Metallurgy, June, 1930, and thus made available to the entire membership. Membership In its report the Admissions Committee set forth the changes in membership during 1929, as follows: Total membership, Jan. 1, 1928, 8582; elected and placed on rolls in 1929, including 59 reinstatements, 509; loss by resignations in 1929, 88; loss by death in 1929, 110; loss by suspension in 1929, 37; membership at end of year not including Student Associates, 8856. Distribution of membership: Honorary Members, 16; Members, 6590; Junior Members, 38; Associates, 1041; Junior Associates, 1033; Rocky Mountain, 138; total membership, Jan. 1, 1930, 8856; Student Associates, 150; total including student associates, 9006. Treasurer's Annual Report, Year of 1929 Statement of Receipts For the year ended December 31, 1929 Dues: Arrears............................................ $ 3,501.75 Current............................................ 97,257.12 New Members...................................... 5,721.50 Advance........................................... 1,970.79 $108,451.16 Initiation Fees.................................................. 7,436.00 Magazine Receipts: Advertising Gross Receipts........................... $40,610.81 Magazine Sales..................................... 3,799.84 44,410.65 Sale of Transactions Current........................... $ 2,985. 15 Sale of Special Editions Current........................ 5,147.82 Sale of Back Transactions and Special Editions........... 4,186.93 Sale of Year Book..................................... 65.50 Sale of Authors' Reprints.............................. 2,585.40 Sale of Pins and Fobs.................................. 14.73 Sale of Technical Publications.......................... 1,451.55 Sale of Bindings...................................... 3,949.13 20,376.21 Net Interest Received: On Bank Balance and Temporary Investments......... $ 2,595.04 On Lie Membership Fund........................... 3,223.43 On James Douglas Library Fund...................... 5,425.61 On General Reserve Fund............................ 2,015.58 13,259.66 Miscellaneous Receipts........................................... 335.80 Total Receipts................................................ $194,269.48

Jan 1, 1930

By Albert L. Toenges

COAL mining technique progressed slowly until the advent of mechanized mining. The cutting machine was a forward step, but had only a limited effect upon improving the percentage of coal recovery. Previously, the physical fitness of the loaders and the total output of the miners fixed mine production. The miner was an independent contractor and supervision over his working place was superficial. Rising costs and the inroads of substitute fuels demanded increased output per man to lower the unit production cost. Therefore, the amount of coal loaded mechanically in underground bituminous mines has risen from 0.3 per-cent in 1923 to 7.4 in 1929, to 20.2 in 1937, and to 48.9 percent in 1943. When loading devices were introduced it became necessary to adapt them to existing systems of mining, or to alter the mining system to fit the machine. An increased amount of supervision was required as output depended upon proper operation of the machine rather than on the physical fitness of the individual.

Jan 1, 1946

By S. Arthur Krom

(New York Meeting, February, 1912.) THE James diagonal-plane slimer is specially adapted to handle the finest slimes, but it will also handle sands as coarse as 40-mesh. The saving efficiency of this machine is due to the original construction of the deck, and to the rapid reciprocating movement imparted to it by the head-motion. The deck consists of a plurality of connected planes, having a certain fixed ratio of inclination one to another. These planes intersect each other diagonally to the stroke-line of the table and are arranged so as to give the pulp on the table a double treatment. This double concentration performed by the diagonal-plane deck produces cleaner concentrates and tailings than those obtained by the operation of two separate machines. The action of the diagonal planes settles, combines, and holds all the concentrates in one compact mass, sharply defined from the gangue, and easily cut away without loss. Many slime-concentrating machines distribute the feed-pulp for a distance of 4 or 5 ft. only, and upon a very limited settling-surface. This results in a thick, heavy deposit, from which it is impossible to stratify the values and wash, away the gangue, the resulting products being dirty concentrates, and tailings carrying high values. The diagonal-plane slimer distributes the feed-pulp for a distance of 10 ft., and upon a settling-surface having an area of 40 sq. ft.; in other words, it spreads the pulp thinly on the table, which allows the metallic values to settle through the gangue quickly, forming a bottom stratum from which the thinly-distributed overlying stratum. of gangue is easily brushed away by the feed-water without disturbing the underlying concentrates. Referring to Fig. 1, plane A is the main settling-section, of the table. The feed pulp flows gently down this plane and is

Jun 1, 1912

By John G. Hall

The unstable metal market during 1949, with resulting lower metal prices, has focused every mine operator's attention on the problem of reducing operating costs. Improvement in mining, methods, use of modern mechanical mining equipment, and increasing the efficiency of the labor force are the tools with which we will have to work. Careful planning is necessary to coordinate all phases so that no one phase is overdone. A mine may become over-mechanized if, for instance, capital charges against new equipment exceed the savings in labor costs, or where a large enough tonnage is not produced. The cooperation, of labor is essential to any mechanization program. There have been too many instances where mechanization and improvements have done nothing more than make up for a decrease in labor efficiency, thus bringing the production of labor back to its old standard. The operator has gained little and labor has gained only a "softer job." In any mechanization program there are gains to be had by both the operator and labor. By the efficient application of modern equipment and improved mining methods the operator should gain by decreased costs, and labor may profit by receiving a share of these decreased costs.

Jan 1, 1950

By Mara Kosovac, Sujan K. Kundu

The Iron Ore Co. of Canada (IOC) has developed a computerized plan analysis method for its open-pit iron mining operations which will eliminate much of the tedious manual drafting of pit design plans performed by engineers and geologists at its two major operational areas near Schefferville, Que., and Labrador City, Nfld. The new technique permits analysis of section or bench plans for a specific ore body, based on drillhole information; preparation of a three-dimensional unit profit matrix for pit design purposes, and storage of extensive ore-block information for other applications. Other advantages include enhanced design accuracy through reduction of human errors normally associated with preparation of large data masses, and by elimination of errors inherent in planimeter-prepared ore block diagrams.

Jan 7, 1978

By A. D. Fernie

Growing interest in pit crushing and conveying is evident from the recent many articles, technical papers, and new equipment development. Application of a pit crushing and conveying system is complex. Many factors, such as mine design, production scheduling, as well as initial and ongoing capital and operating costs must be thoroughly and realistically examined. This paper will address the fundamentals to be considered and review several approaches to developing a total system for a new and existing mine situation. The planning function will be outlined and operating and design criteria defined to interface the mining operation and the pit crushing conveying system.

Jan 1, 1986

By Harold Price

PRIOR to Sept. 1, 1928, there had never been constructed what might be termed a long pipe line with electric-welded field joints. Nevertheless, by Sept. 1, 1929, within the period of a year, more than 2500 miles of electric-welded lines have been completed. These lines vary in diameter from 6 to 20 in., and in length from 50 to 700 miles. Before Sept. 1, 1928, no such line had been constructed .longer than 50 miles, and only one of nearly that length, a 40-mile 7-in. gas line in Louisiana. This was in reality the first pipe line to use electric-welded field joints. During the past year the following lines have been electric-welded by the Welding Engineering Co. alone: Texas Pipe Line Co.-157 miles of 8-in. line from Corsicana, Texas, to San Augustine, Texas. (This was the first electric-welded oil line.) Texas Pipe Line Co.-80 miles of 8-in. from Lafors, Texas, to Childress, Texas. Texas Pipe Line Co.-39 miles of 10-in. from Monahans, Texas, to Jal, New Mexico. Texas Pipe Line Co.-50 miles of 6-in, from San Antonio, Texas, to San Marcus, Texas. Texas-Empire Pipe Line Co.-424 miles of 12-in. from Cushing, Okla. to Chicago, Illinois. In addition to the field welding mentioned above,1 250 miles of 12-in. line was electric-welded into double joints at the pipe mill at Indiana Harbor, Ind.

Jan 1, 1929

By Edgar T. Wherry

EDGAR .T. WHERRY,* Washington, D. C. (communication to the Secretary ?).-Dr. Pogue's presentation of the facts concerning the emerald deposits is very clear and convincing, and the only addition that I can suggest is a summary of previous theories of origin. He makes it evident that the pegmatite theory is the only one capable of explaining the existing relations, but upon certain details there may be some difference of opinion. If I understand the term pneumatolytic, it does not imply that all the elements concerned in a given deposit were transported as gases, but rather that the crystallization of these elements into the various minerals was favored by the presence of certain gaseous substances, notably H20, C02 and HF. It is highly improbable that the oxides of glucinum, aluminum, chromium, and silicon, which enter into the composition of the mineral emerald could have been transported in the gaseous form. The same is true of the metallic constituents of the parisite and other associated minerals. The explanation suggested, that solutions separated into liquid and gaseous portions, the latter ascending and forming the emerald in the upper portions of the rock only, therefore, seems to me untenable. When two formations exist side by side and one, A, is mineralized while the other, B, is barren, the possible explanations may he classed as (1) chemical, and (2) physical. 1. Some chemical feature of A not found in B might have caused crystallization of certain minerals in the former, which did not appear in the latter. In the present instance both rocks appear to be so similar chemically that no such effect can be looked for. Pogue mentions carbon as a possible precipitating agent, but describes both formations as carbonaceous, so that the difference in the minerals of the two can not be thus explained.

Jan 10, 1916

By Francis Lucas

ANY metal which contains even a small percentage of aluminum possesses certain peculiarities of appearance and properties which are exhibited both when the metal is melted and after it solidifies. Pure aluminum, or an alloy containing a small proportion of aluminum, can be melted without flux-except for a layer of charcoal-because a film of aluminum oxide and metal forms at the surface of melted aluminum. Although very thin, this film is air-proof, and it prevents the metal underneath from oxidizing. This oxidized film does not move easily on account of its toughness and high surface tension. One very important point in connection with this process of still casting has not been strongly enough stressed, namely, that the same kind of surface film with the same peculiarities forms over the surface of all melted alloys that contain even a small proportion of aluminum. Experienced foundrymen know how desirable it is to cast aluminum under its "skin" or-under the surface of the film which tends to remain still. In the case of red copper, when in fusion, the surface shows pure copper only. This is due to the fact that liquid copper constantly absorbs the copper oxide which forms on the surface. By closely examining melting copper the oxide can be seen dissolving in the bath, and going into solution just as pulverized sugar dissolves in water. When copper is cast in the open, either in wire bars or cakes, the surface of metal exposed to the air is covered by a film of black, oxide that cannot be absorbed by the metal.

Jan 1, 1927

By J. Groyecki, M. Markuszewicz, J. Lassota, A. Zawada

The ratio of stable to unstable inclusions was found to ploy an essential role in the process of sccorldar-y recrystatlizalion in Si-Fe. The analysis of the free energy of inclusions in the range of heat-treatment of individual inclusions to be predicted. The effects MnS. ns inslable inclusions. were investigated. TO secure a high induction, the secondary recryslulliztt-lion associated wilh the texture is necessary. To obtain a low core loss an additional refiuing in the solid state is required. It has been found that sulfur can be more easily removed in racunm than in hydrogen and thai this process was hindered by the prescrzce of INCLUSIONS play an essential role in the development of cube-on-edge texture in Si-Fe. Their function consists in restraining the growth of primary grains up to about 900°C and in passing subsequently into solution at higher temperatures. This process is accompanied by the selective growth of secondary grains with (110)[001] orientation. The general effect of inclusions depends on such factors as the type of impurities, their amount. dispersion and stability, the conditions of diffusion in the space of lattice of metal, and the reactions at the metal/gas interface. In recent years, some of these factors were the subject of a special investigation. A positive influence of Mns, siN,' and vN3 has been established. The quantity of impurities4 and their dispersion5 have been found to be of major importance. Attention was called to the vital importance of diffusion and the conditions under which the impurities are removed from metal., It has also been demonstrated that in Fe-Si alloys by the techniques of powder metallurgy a special opportunity exists to obtain the (110)[001] type texture. 6 The aim of this work was to conduct qualitative investigations on the influence of inclusion stability on the development of cube-on-edge texture in a metal containing approximately 3 pct Si. Experiments were carried out on cast alloys and on those manufactured by powder-metallurgy techniques. The results obtained from these experiments were utilized to explain the phenomena involved and to analyze the relationships between stable and unstable inclusions and the magnetic properties of alloys. EXPERIMENTS AND RESULTS The raw materials used in these experiments were the powder of carbonyl iron with the analysis (in pct) 0.044 C, 0.01 Mn, 0.005 Si, 0.009 P, 0.002 S, traces of Cu, 0.06 Ni, 0.0015 Al, 0.03 Cr, 0.02 Mo, 0.01 Ti, 0.002 Co, traces of Pb, and the powder of silicon containing 94.14 Si, 0.003 S, 0.048 C. The powders were ground and mechanically mixed in 100-g batches. and then pressed at 9 tons per sq cm into 74 by 24 by 8 mm blocks. Sintering was carried out at 1100°C for 12 hr in vacuum (2 x lo-' Tr) or in hydrogen. In this instance the material was heated slowly and subjected to prolonged soaking at 350°, 650°, and 750 2C, respectively, to secure reduction of ferro-oxides. This was checked by making measurements of the dew point, which was found to change from -15" to -35°C after reduction. The compacts after sintering were hot-rolled to 2.4 mm, annealed at 800 C, and finally cold-reduced to 0.35 mm with intermediate annealing at 800°C at a gage of about 0.8 mm. Impurities were added in the powdered form and mixed with iron and silicon powders. Sulfur in the elemental state, electrolytic manganese, and pure aluminum oxide were employed. Besides, to obtain a material with low contents of impurities, especially

Jan 1, 1967

By R. R. Harvey

Recent evidence has indicated that the films forming at crude oil-water interfaces are the result of naturally occurring su,rface-active components in the crude oil rather than oxidation products resulting from exposure of the oil to air. Since the presence of such films may strongly affect the displacement of oil from porous media, a knowledge of their composition and formatiorz is of fundamental importance. In this study, without the assumption of a specific mechanism, film formation is considered to involve the transfer of a weakly surface-active species in solution in the oil to the oil-water interface. The film gas law and the Gibbs adsorption equation may thus he applied to the system. The rigid films which form upon decrease of the oil-water interfacial area are considered a result of the very slow rate of re-solution of the film material into the oil. When the shrinkage of the interface is very rapid, the amount of film material leaving the interface is negligible, and the system may then be treated in the same manner as an insoluble film. The combination of these treatments leads to a new concept of the film factor in which it may he quantitatively related to the concentration of film-forming material at the interface. Suitable experiments can then yield the following information. 1. Original concentration of surface-active species in the oil. 2. The change of concentration with time. 3. Concentration of surface active species at the interface. 4. The change of this concentration with time. 5. Interfacial tension of the system at any time and its variation with time. 6. Equilibriunz concentrations for a given set of conditions. 7. Concentration requirements for solid film formation. 8. Molecular diameter of the adrorbed species. These calculations may be made solely from data taken from measurements on the original oil. While using the pendant drop method of interfacial tension measurement of crude oil-water systems, Bartell and Niederhauser' remarked on the thin, transparent, pliable, solid films or membranes which were often formed at the interface between crude oil and water. As a result of their observations of these films, Bar-tell and Niederhauser concluded: 1. The films are formed by material from the oil adsorbed at the interface rather than by a reaction at the interface. 2. The adsorption of the film-forming material is a rather slow process. 3. There are good indications that the process is reversible; i.e., the film constituents may re-dissolve into the oil. 4. The film will spontaneously spread over any new surface formed. 5. The process of adsorption at the interface is accompanied by a decrease in the interfacial tension of the system. Although they had proved that film formation was not due to a reaction at the interface, Bartell and Niederhauser were unable to demonstrate conclusively whether these film-forming constituents were present in the original reservoir oil or whether they were formed as oxidation products after exposure of the oil to air. Recent evidence seems to point to their presence in the original oil. Although the true nature of the film-forming constituents is still uncertain, these conditions would be fulfilled by the assumption of the presence of a slightly soluble surface-active component in the original oil. This component would migrate to a freshly formed interface because it would thereby lower the free energy of the system. The component at the surface constitutes an expanded monolayer which would become compressed, upon retraction of drop, due to the slow rate of re-solution of the film components into the bulk of the oil. It is possible, by involved extraction processes, to separate or at least concentrate this film-forming fraction. However, using the assumptions made above, the technique of monolayer film study may be applied to reveal much of the nature of the adsorbing material without resorting to an actual separation of the film-forming constituents.

By P. CHARTERIS A.

THE following scanty notes on the Roumanian oil-region may serve as an introduction to more detailed future study and description. The Roumauian oil-belt, follows the outer edge of the sweep of the Carpathian Mountains, and may, in a broad sense, be regarded as a prolongation of the Galician belt. It is distributed over a tract of country from 300 to 400 miles in length, with a width of from 15 to 20 miles, and is believed to cover an area of at least 20,000 hectares (59,420 acres). The Government claims that 16,000 to 17,000 hectares of its land is petroliferous. The primary deposits of petroleum are considered to be in the Padeogene (Oligocene) and the Neogene (the salines of the Miocene) formations. Most of the other repositories, especially those of Muntenie, are only secondary, the petroleum there having been introduced by the orogeneric movements which raised the Carpathian Mountains. The oil-field has been divided by the Roumanian survey into two regions, the Flysch and the Sub-Carpathian, as is shown in the accompanying sketch-map, Fig. 1.(p. 518). So far as is yet, known, practically all the seepages and .productive pits and wells are situated oil anticlinals. Those which outcrop in the Flysch region. (called Paleogene anticlinals), as indicated in the sketch-map, Fig. 1, are : Solontz, Middle Oligocene; Moineshti, Moineshti and Tagu-Ocna-beds of the Eocene.

Jul 1, 1906

By Franklin G. Pardee

WARTIME depletion of the reserves of iron ore in the Lake Superior region of the grade and character now being shipped down the Lakes was serious. The time has come to take stock of the resources that remain in order to plan our future program of supply for our blast furnaces and protect, as far as possible. the tremendous investment made in the Lake Superior iron mining industry. Hugh M. Roberts and William H. Crago have estimated the reserves of the Lake Superior region in the United States at two billion long tons. These reserve figures are of direct-shipping ore and those concentrates produced by methods now in commercial use or those methods that may be expected in the near future. In their estimate they have assigned 392 million long tons to the Michigan ranges (all reserves in long tons) : 112 million tons for the Gogebic. 140 million tons for the Menominee, and 140 million tons for the Marquette.

Jan 1, 1948

By R. H. Pemberton

The principle of airborne electromagnetic prospecting is well-known. The basic geophysical texts in most cases discuss the main elements involved in electromagnetic prospecting. However, there is certainly little information available to the public concerning the present types of airborne electromagnetic systems being flown today by both contracting companies and some of the mining companies which have their own instruments. This is unfortunate since it is difficult for those people not conducting such operations to understand thoroughly the large variation in the electromagnetic instruments available.

Jan 1, 1961

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 R. B. Fuller, E. T. Casler

MANY changes were made in the methods and equipment used in the mining of pebble phosphate rock in the generation immediately preceding the present World War and it would be extremely interesting to note the improvements that will be made during the next generation. Literally, much water has gone over the dam since the days when we used local cordwood for generating steam and drying pebble phosphate rock. belt-driven centrifugal pumps operated by steam engines. and floating dipper or centrifugal dredges; when we removed overburden by small steam shovels and transported it by dinkey locomotives and six-yard cars; when washing machinery was installed on wooden structures the washers being replaced every four to six years. Those were the days when men were plentiful, and 47 different mining companies were selling their products, based on .decidedly meager information; and. like so many mining operations, little thought was given to conservation. As the importance of phosphate rock has become more prominent in the thoughts of our economists, a more intelligent approach has been made to mining problems. Vast improvements have been made in the technique and processing of the phosphate matrix and stripping of overburden, which, in turn, have brought developments in machines and equipment and a more

Jan 1, 1944

By A. W. Ambrose

THE underground losses of oil exceed by hundreds of thousands of barrels all the oil that has been lost in storage, transportation, or refining. The quantity lost is, of course, indeterminate; but when it is considered that the contents of an entire oil field have been excluded from recovery by invading waters, some idea of the amount wasted may be gained. Similarly, enormous quantities of gas have been lost underground. Conservation of the oil, therefore, should start before it is brought to the surface rather than after it is placed in storage tanks. Water is one of the most important causes for underground losses and the operator should give as serious consideration to an underground flood of water as he would to a destructive surface flood. The best insurance, of course, is to have the wells drilled in such a manner that water has no access to the productive oil and gas horizons, and on abandonment the wells should be properly plugged. The encroachment of edge water and the occurrence of water in the base of an oil sand present a very serious problem to an oil company; sooner or later these waters are bound to cause considerable damage, if they do not entirely destroy the possibilities of further production. Too often, however, a field has been considered to be in a hopeless condition, whereas wells in as bad a condition in other areas have been repaired and the life of the field appreciably lengthened. The corrections are very often suggested by technical study. Very successful results have been accomplished by detailed underground work in the California oil fields, in Cushing, Oklahoma, and in other areas.

Jan 9, 1920

By Albert Brokaw

THE so-called ?paraffin dirt" of the Gulf Coast oil fields has been con¬sidered an indication of the possible presence of oil and gas, and not a few wells have been brought in solely on the basis of such evidence. In a sense, it may be empirically justified as evidence of the presence of oil or gas, though it cannot be said to be infallible. If the writer is correctly informed, its association with oil and gas was pointed out by Lee Hager some years ago, and while it is commonly mentioned by geologists and operators in conversation, no discussion seems to have found its way into print. The present interpretation is based on laboratory study rather than on field investigation, and is put forth with the hope of stimulating discussion which shall lead to more complete understanding. The term "paraffin dirt" has been applied to soils with a peculiar texture, which has been described' as "curdy" or "rubbery." When moist, the material breaks much after the fashion of "green" cheese. It is rubbery under compression, but does not resemble rubber in tenacity or cohesion. When dry, the material ranges from hard clods to a horny mass of high tensile strength. The shrinkage in drying is very great, especially in the hornlike matter. The moist material ranges in color from dark brown in the specimens rich in organic matter to grayish in specimens containing more inorganic matter. All of the specimens studied were readily attacked by molds, which in some cases grew in great profusion on the samples. Samples exhibited a rather characteristic "swampy" or "mucky" odor when wet, and a characteristic odor of humic soils when moist.

Jan 4, 1918

DISCUSSION, M. Cohen presiding A. H. Geisler and D. L. Martin (GeneTal Electric Research Laboratory, Schenectady, N. Y.)—We were rather interested to note the author's conclusion that the cubic to tetragonal transformation may be of the second order, for we have been able to show that the order-disorder transformation in an analogous alloy system is a first-order transformation with a discon-

Jan 1, 1952

By R. P. Abendroth

This study is concerned with the kinetics of selective oxidation of chromium in a commercial Fe-Cr-Ni alloy. Selective oxidation of chromium in this alloy, by use of a low oxygen-potential atmosphere, leads to the formation of a compact, protective layer of Cr2O3. This layer serves to protect this alloy from gross scaling when it is subsequently exposed to severe oxidizing conditions at high temperature. The interaction of low oxygen-potential atmospheres close to equilibrium with Fe-Cr and Ni-Cr alloys has been studied by others."' These studies werk concerned with the surface-structure variations under slightly oxidizing conditions. NO detailed study was made of the oxide scale formation kinetics, however. The alloy samples were cut from 0.012-in.-thick sheet, with an apparent surface area of 7.1 sq cm. These sheet samples were abraded through 4/0 metallographic paper, and washed in alcohol and acetone. The analysis of the sheet alloy is (in weight percent): 42 pct Ni, 5.5 pct Cr, 0.09 pct C, 0.18 pct Al, 0.36 pct Si, 0.26 pct Mn, balance Fe. The weight gain vs time data were obtained with a 2-g capacity fused-silica spring—cathetometer system. The spring deflection was optically magnified ten times before being read by the cathetometer. A sensitivity of about 0.01 mg was attainable. The spring was enclosed in a water jacket maintained at 60°C to minimize the effect of temperature changes. The sample was suspended from the spring with a fused-silica hangdown and was positioned in the thermal center of a mullite furnace tube. Sample temperature was read with the aid of a thermocouple placed outside the mullite tube and an inside vs outside temperature calibration. Temperature change during the course of a run was ±0.25°C, with a temperature gradient of less than l.O°C over the length of the sample. Total temperature uncertainty was no more than ±3.0°C. Alignment difficulties between the hangdown and radiation shields in the furnace tube required that the sample be positioned in the furnace when cold, and heated with the furnace until the temperature stabilized at the desired point. This required 5 to 6 hr, and was carried out in Matheson ultrahigh-purity hydrogen. Oxidation was started, after evacuation, by introducing a hydrogen-water vapor mixture, obtained by saturating hydrogen with water vapor at 31.00o ± 0.02oC. Oxidation was continued for 90 min. Gas flow was 300 ml per min during heat up and oxidation. Since only several milligrams of oxide are formed on each sample, chemical analysis of the oxide is difficult. A representative analysis is: 80 pct Cr2O3, 5 pct Fe2O3, 3 pct Al2O3, 4 pct MnO, 7 pct SiO2, 1 pct or less NiO. X-ray diffraction analysis of the oxide as formed on the alloy gives rhombohedra1 Cr2O3, and barely distinguishable amounts of a cubic spinel phase, and possibly AlZOs and SO2. The identification of these latter two compounds is by no means certain. The spinel phase could be based on iron or manganese as these elements are present in significant amounts in the oxide. The results of the kinetic studies using 31°C dew-point hydrogen-water vapor mixtures were found to conform to a parabolic rate law. In many cases the parabolic plot consisted of two intersecting straight lines, defining an early and a late rate for a particular run, and in the other cases the parabolic plot consisted of one straight line for the entire run. The slopes of the various straight lines were determined by the method of least squares. Reproducibility of the data was good enough for multiple runs at the same temperature such that the value given for the rate constant is the average for two or more closely similar values, rather than widely varying values of the rate, where more than one determination is indicated in Table I. The exhibition of only one or of two rate constants during a run can happen at the same temperature. Thus, Table I shows that at 11'74°C a single rate constant was obtained from one sample, while other samples oxidized at the same temperature gave an early and a late rate constant. It should be noted that the single rate constant corresponds very closely with the early rate constant. This is also true at 1153°C. The time at which the late rate started to appear was variable, usually occurring 20 to 40 min after oxidation had started.

Jan 1, 1964