Search Documents

By A. U. Seybolt

RECENTLY, cases of coexisting ordered and disordered phase equilibria have been reported among face-centered cubic metals,1"3 but not on body-centered cubic systems.4 McQueen and Kuczynski5 showed a single line as the boundary between ordered solid solution of Fe3Al type and corresponding disordered solution in the Fe-A1 phase diagram based mainly on dilatometric and magnetic measurements. Such a single line would indicate a second or higher order transition. or an absence of coexisting order and disorder. The writer found previously a two-phase equilibrium region at 800°C consisting of ordered and disordered solid solutions of Fe3Si in a matrix of approximately 1-6 wt pct Si (Fe3Si is of 14.3 wt pct Si). A similar two-phase region of ordered and disordered Fe3Al solid solutions might be expected if the similarity between Fe3Si and Fe3Si structures hold true. In the present investigation, a wire of 22 at. pct Al, balance Fe and 0.0513 cm in diameter was subjected to electrical resistivity measurement in vacuum as a function of temperature between 300 and 800°C, see Fig. 1. There was excellent agreement between data taken on heating and on cooling: no hysteresis was observed. The Curie temperature was determined to be 640 °C which agrees with the finding by McQueen and Kuczynski.5 But in addition, there were two transitional points in the resistance-temperature plot at 510oC and 400 "C. The former is thought to be a connection with the transition from disordered state to a coexisting order and disordered equilibrium state; while the latter, from such coexisting state to ordered state. Fig. 2 shows a phase diagram where the suggested two-phase region lies between dotted lines. The solid lines are those of McQueen and Kuczynski.5 Since these authors found only a single-phase boundary between ordered and disordered Fe3 Al, it would seem likely that the dilatometric method used by these authors was not sufficiently sensitive to resolve the ordering reaction into the two-phase boundaries. In addition, their phase diagram conflicts with the statement they make on P. 1 of their paper: "The sharpness of the peaks indicates that ordering to Fe3A1 is a first order reaction." The suggestion of coexisting order plus disorder in Fe3A1 must be considered tentative until confirmed by high-temperature X-ray examination. If

Jan 1, 1961

By J. Laskowski

J. Laskowski (Associate Professor, Dept, of Mineral Processing and Coal Preparation, Silesian University of Technology, Gliwice, Poland) -Referring to the papers by J. A. L. Campbell and S. C. Sun, I must say that I am very pleased to see that type of work, because it is the only way to progress towards an understanding of flotation mechanisms. All those interested in the science of the surface chemistry of coals would find these papers a valuable contribution to the literature. In their extensive research, the authors attempt to synthesize their findings into a theory of coal flotation. To do this, the zeta potential of bituminous coals and their lithotypes, as well as that of an anthracite coal, was measured and H+ and OH- ions were found to be potential determining ions. The measured ZPC of bituminous coals was at a pH range from 3.5 to 4.6 and for the anthracites between 2.0 and 4.5. The authors have pointed out that since the hydrophobicity is pH-controlled, the flotation mechanism should also be. The Campbell and Sun papers confirm a good many of the conclusions on surface properties of coals reported in recent years. It is noteworthy to point out that the ZPC found in the paper on bituminous coals was approximately pH 4, similar to the ZPC for the anthracite coal. In fact, we have been investigating different coals from low to high ranks. Thus, the plot of the pH for ZPC against rank could be derived and this curve-an electrocapillary one-indicates a pH near which the hydrophobicity of the coal surface should be at maximum. This can be proved by so-called salt flotation, which, in a sense, can be treated as method of surface charge measurement. It is obvious that the salt flotation experiment is possible when the native hydrophobicity of the mineral surface is high, e.g., when the solid surface does not have an orienting influence on an adjacent water layer and the hydration layers are controlled by the electrical double-layer potential. The addition of electrolyte or a change of pH which decreases the thickness of the stabilizing double-layer "opens up" the hydrophobic surface micro-area mosaic. Thereby the surface becomes hydrophobic and particles become floatable. The orienting influence of surface on hydration layer increases even after very slight oxidation and flotation is affected by it. It seems that such an explanation agrees reasonably well with those of Campbell and Sun.

Jan 1, 1972

By Jean Howard, E. V. Walker

ManY papers have been published during the last few years on the formation of cube texture in 3 1/4 pct Si-Fe, e.g., those of Assmus, Detert, Dunn, and Walter.1,5 All are concerned with the formation of the texture by a process involving secondary re-crystallization and the relative surface energies of (100) and other planes under certain conditions of annealing. The authors have found that cube texture can also be produced by heavily cold rolling strip in which the cube-on-edge texture has first been formed. Cube texture develops on annealing, but in this case it is not accompanied by secondary recrystallization. The starting material is a sintered compact, the preparation of which has been described elsewhere. Using a conventional processing schedule employed for producing commercial silicon-iron with the cube-on-edge texture, the sintered compact is cold rolled to such a thickness that, after annealing in pure hydrogen for 24 hr at 1350'~ to produce the cube-on-edge texture, the final thickness required can be obtained by giving a further cold reduction of 85 pct. Cube texture is developed by annealing at -900~~ in pure hydrogen: it has been produced in strip up to 0.024 in. thick. The microstructure of the strip consists of a mass of small primary grains within the boundaries of the much larger secondary grains which ex- hibited cube-on-edge texture before the final cold roll. If the strip is annealed at -1000 after the 85pct reduction, secondary recrystallization begins to take place, provided a strong cube texture is present. On raising the temperature more secondaries grow, complete secondary recrystallization being obtained on annealing at -1150'. From this it is concluded that the secondary crystals are produced by the texture inhibition mechanism: they show (110) and (111) planes in the surface of the strip, the former being the more numerous. It has been observed that the more perfect is the (110) [001] texture prior to cold rolling by 85 pct, the further from the ideal is the (100) [oo].] texture. A similar treatment applied to high quality commercial grain-oriented silicon-iron strip failed to produce cube texture. The tilt and rotation of the [loo] from the rolling direction was less than 10deg, but (to within a few degrees) the planes (130), (450) and (210) lay in the surface of the strip. Acknowledgment is made to the Engineer-in-Chief of the British Post Office for permission to use the information contained in this note.

Jan 1, 1962

By J. B. Cohen

In an investigation of the microstructure of shock-loaded metal specimens1 C. S. Smith found that there was little distortion of grain boundaries or change in external dimensions, although the hardness corresponded to that produced by severe rolling. Furthermore, the hardness of individual grains was independent of the deformation structures present; grains with no markings were as hard as those heavily populated with markings. These markings which resemble twins do not appear in copper until high shock-loads of the order of 200 kb are applied. It appears that due to the high velocity of a shock wave and its sharp front, heavy deformation takes place on a submicroscopic scale. In this work an attempt was made to examine this deformation, particularly at a load below which macroecopic markings appear. The broadening of 200 and 400 diffraction peaks was examined from the face of a poly crystalline sample normal to the direction of the shock wave. These peaks were chosen because the elastic constants in copper are such that residual strains would be greatest in the <100> directions; hence, the strain-broadening contribution to these peaks would be large in comparison to other sets. Also the broadening due to stacking faults and microtwins would be greatest with this set.2 A complete Fourier analysis of these peaks was made, as described by warren,&apos; using the Stokes correction with peaks from an annealed sample.3 With the aid of the U. S. Army Ordnance Corps EDVAC computer and a curve matching program, sixty sine and sixty cosine coefficients were obtained for each peak. The last of these was about 1.5 pct or less of the largest coefficient, indicating good representation. Transverse sections from a 1.5 in. rod of as-drawn electrolytic tough-pitch copper were reduced in cross-sectional area about 50 pct by cross rolling. Disks 1.5 in. in diam were recrystallized at 275 °C for 30 min and then at 300°C for the same time. The faces were polished and deeply etched in nitric acid to remove 25 mils. The grain size was 0.02 mm. Laue back-reflection patterns indicated the sample was well recrystallized. The two diffraction peaks from this sample were recorded on a Norelco diffractometer using filtered copper radiation. Peak intensities were kept less than 600 cps to assure linearity of the counter and circuitry. This sample was then placed between two rods of the same material and diameter. The top rod was 2.25 in. long and the bottom rod 1 in. long. (In

Jan 1, 1961

W. D. BRENNAN,* Cheyenne, Wyo. (written discussion?).-My experience has been that, where possible, it is preferable for each foreman to employ his own men, rather than to have them handled through an employment bureau. The fact that each foreman comes into direct contact with the man before he is put to work gives him an opportunity to choose, at certain times, the kind and class of men that he wishes. Where possible, after a man is employed he is sent to a central office where a complete history of each individual is kept on a card. If a man has previously been in the employ of the Company, his history can be obtained from this card, and if for any reason he is not wanted he can be refused work at the time he reports to, the central office. In connection with Workman&apos;s Compensation costs, we in Wyoming feel that although the rates of compensation paid may in some cases be rather low our law works satisfactorily. As the State and the number of employees are small, compensation cases are handled through Judges of the various District Courts. In the State Treasurer&apos;s Department, a few clerks were added to look after the handling and issuing of warrants and compiling of statistics. Most of the large employers have an arrangement by which a joint claim and assent, specifying the amount of compensation due, is made tip by the employer and signed by the workman. This is forwarded, to the Judges so that personal investigation of individual cases is not necessary. In this manner, compensation is promptly received and&apos; overhead expenses of operation of the law is kept at the minimum. The law requires each employer to pay into the State Treasury, for the benefit of the industrial fund, a sum equal to 1.5 per cent. of the money earned by each employee, engaged during each calendar month of such employment. Each employer contributes monthly, unless the sum heretofore contributed, after deducting all payments made on account of injuries to his employees, shall equal a full 1.5 per cent. of his annual pay roll, computed by multiplying his current monthly pay roll by twelve, and shall likewise be not less than ($5000). It has been found during the years that this law has been in effect, that a number of the larger employers have been exempt from payment for from five to eight months per year, so that in some cases, even in coal nines, industrial insurance has cost less than 0.75 per cent.

Jan 3, 1919

By E. C. Franz

IN an effort to understand high cycle fatigue, as well as to study the mechanism of fracture in general, a number of researches have been undertaken whereby the fracture properties of a metal have been determined under conditions of repeated cyclic prestsain employing high strains with relatively few cycles. Liu, Lynch, Ripling, and Sachs&apos; showed the effect of a definite strain history consisting of small increments of tensile or compressive prestrain upon the flow and fracture characteristics of metals after a limited number of repeated loadings. Liu and SachsW emonstrated by cyclic straining of the aluminum alloy 24s-T4 that the least reduction in ductility was obtained when the compressive stress was nearly equal to the tensile stress. Attempts have been made to correlate the reduction in ductility under such prestraining with conventional fatigue data, as was done by Liu and co-workers.&apos; The following research was conducted to determine if such reduction as has been noted could be correlated with conventional fatigue data or whether the effect resulted from causes extraneous to the basic mechanism of fatigue failure such as strain aging. It might be pointed out in this connection that the reduction in ductility has occurred in alloys that might be susceptible to strain aging or similar behavior, such as alloy 24s-T4. In the present investigation, the test specimens were prepared from the aluminum alloy 75s-T6 and annealed electrolytic copper. Alloy 75s-T6 is a complex precipitation hardenable alloy, whereas electrolytic copper would not be expected to exhibit strain aging effects, particularly at room temperature. The experimental procedure consisted of prestraining test specimens repeatedly by increasing tension in small increments to various total prestrain values, followed by testing to failure in a tension test. The prestraining as well as the final testing was performed on a tensile machine using special fixtures9 0 maintain concentricity of the specimens. After prestraining, the specimens were unloaded as rapidly as possible and immediately reloaded so that the total time lapse between strains was held to a few seconds. Logarithmic or true natural strain was used in all calculations. The results are presented in Figs. 1 and 2. In Fig. 1, the retained ductility, area after prestrain area at fracture is plotted against the tensile prestrain, initial area area after prestrain as abscissa with the number of stress reversals executed to attain the required prestrain plotted as parameter. Several specimens that fractured during

Jan 1, 1955

By William Kent

In a paper by Mr. Frank Firmstone, published in vol. iv, of the Transactions of the Institute, on " Comparison of Results from Open-topped and Closed-topped Furnaces," the regularity of the average grade of pig iron procluced by the furnace under different conditions is expressed by means of a curve or diagram. The object of this note is to show that the graphic method, or that of representing variations by plotted curves or diagrams, is capable of a much more extended application to blast-furnace records, making a valuable auxiliary to the " furnace hook," and that by it the practical metallurgist may obtain at a glance information concerning the variations of the furnace during long periods, which could be found in the furnace book only after a tedious search. Plate XII is a graphic record of an anthracite blast furnace for one month. The table on page 554 gives the figures obtained from the furnace book, together with a record of temperature of the atmosphere, barometric pressure, and moisture in the air, which was obtained from a meteorological observatory not far from the furnace. In the records of a furnace, two of the variable qualities are final results, viz., the quantity of pig iron produced, and its grade; all the other variables are antecedent causes which produce the final results. Of these variable callses which contribute to the quantity of product and its grade, some are partially under the control of the furnace manager, others depend upon the state of the atmosphere, and still others are accidental. Of the first class are the character of the materials charged, and their relative proportions, their mechanical conditions, as wetor dry, large or small pieces, etc., the revolutions of the engine, the heat and pressure of blast, and the distribution of the charge. Of the second class are the number of pounds of air blown into the furnace for each stroke of the engine, the amount of moisture in the air, and the condition of the chimney draughts. These vary largely with the season of the year. Of the third class is the leaking of a tuyere or a temporary stoppage. To keep a record of this kind for a whole year, it is only necessary to procure a sheet of common profile or cross section paper, about 38 inches long and 8 or 10 inches wide, with cross lines ruled about 0.1 of an inch apart. The vertical lines, or those in direction of the

Jan 1, 1879

By William Kent

(Read at the Amenia Meeting, October, 1877.) IN a paper by Mr. Frank Firmstone, published in vol. iv, of the Transactions of the Institute, on "Comparison of Results from Open-topped and Closed-topped Furnaces," the regularity of the average grade of pig iron produced by the furnace under different conditions is expressed by means of a curve or diagram. The object of this note is to show that the graphic method, or that of representing variations by plotted curves or diagrams, is capable of a much more extended application to blast-furnace records, making a valuable auxiliary to the "furnace .book," and that by it the practical metallurgist may obtain at a glance information concerning the variations of the furnace during long periods, which could be found in the furnace book only after a tedious search. Plate XII is a graphic record of an anthracite blast furnace for one month. The table on page 554 gives the figures obtained from the furnace book, together with a record of temperature of the atmosphere, barometric pressure, and moisture in the air, which was obtained from a meteorological observatory not far from the furnace. In the records of a furnace, two of the variable qualities are final results, viz., the quantity of pig iron produced, and its grade; all the other variables are antecedent causes which produce the final results. Of these variable causes which contribute to the quantity of product and its grade, some are partially under the control of the furnace manager, others depend upon the state of the atmosphere, and still others are accidental. Of the first class are the character of the materials charged, and their relative proportions, their mechanical conditions, as wet or dry, large or small pieces, etc., the revolutions of the engine, the heat and pressure of blast, and the distribution of the charge. Of the second class are the number of pounds of air blown into the furnace for each stroke of the engine, the amount of moisture in the air, and the condition of the chimney draughts. These vary largely with the season of the year. Of the third. class is the leaking of a tuyere or a temporary stoppage. To keep a record of this kind for a whole year, it is only necessary to procure a sheet of common profile or cross section paper, about 38 inches long and 8 or 10 inches wide, with cross lines ruled about 0.1 of an inch apart. The vertical lines, or those in direction of the

Jan 1, 1878

By Irving Cadoff, Jack Medoff

THE linear thermal expansions of oriented single crystals of zinc were measured in the range from 20" to 416°C using a Leitz HTV optical lever differential dilatometer. The single crystals, supplied by Dr. J. J. Gilman, General Electric Research Laboratory, Schenectady, N.Y., were prepared from 99.999 pct-purity zinc, and were in the form of rods approximately 2 in. long by 0.15 in. in diameter having the following orientations: x = 1.5, 12, 20, 30, 37.5, 49, 60, 73, and 82 deg where x is the angle between the specimen axis and the (0001) plane of the crystal. From the family of expansion vs temperature curves, the instantaneous expansion coefficients were calculated at 100°C intervals, and Fig. 1 shows a plot of these derived coefficients for each orientation. Coefficients were obtained from the raw data using the chord-slope method. The curves in Fig. 1 indicate a positive temperature coefficient for low x, a negative temperature coefficient for high X, and an expansion coefficient invariant with temperature, amounting to about 43 x 106, for a crystal orientation of approximately 52 deg. From the available data, it is possible to arrive at the values for the axial thermal-expansion coef- ficients a, and a, by extrapolating the curve of the expansion coefficient vs orientation to zero and 90 deg orientations. More precise values for a, and a, are obtained if the instantaneous coefficients are plotted against the square of the cosine of the orientation angle, as shown in Fig. 2. The extrapolated terminal points of the best straight line through the data points of such a plot define the axial coefficients at that temperature. The theoretical justification for the linearity of this curve comes from inspection of a rearranged form of the general anisotropic equation for expansion: ax=a, + (a, -a,)cosZx [1I in which a, is the expansion coefficient in the "c" or [0001] direction and a, the expansion coefficient in the "a" or [ll50] direction. From Fig. 2, the axial coefficients at 100°C, for example, were found to be a, = 13.9 x 10&apos;6 and a, = 62.4 x 10"6 per "C. In the same way, the coefficients were determined for 20", 200°, 300°, and 400°C. This data is summarized in Fig. 3. It is of interest to observe the common intersection of the curves in Fig. 3, which seems to bear out the earlier observation, from Fig. 1, of a

Jan 1, 1964

By W. H. HOWARD

Discussion of the paper of W. H. HOWARD, presented at the Salt Lake meeting, August, 1914, and printed in Bulletin No. 92, August, 1914, pp. 2029 to 2046. EDGAR M. DUNN, Anaconda, Mont.-Mr. Howard&apos;s contribution to the literature on the Cottrell, method. of electrostatic precipitation of flue dust and fume at Garfield has been read by us with peculiar interest for the reason that we have been experimenting with the same process at Anaconda for the past eight or nine months, with a view to adapting it, under the direction of Dr. Cottrell and the supervision of J. 0. Elton. and D. R. Kellogg, representing the Anaconda Smelter Commission, to the treatment of very large volumes of gases, using large pipe treaters and various forms of electrodes, with about 150,000 volts rectified current. For the amount of gas to be treated here the 5-in. pipe means a cost for installation that is practically prohibitive, clue to the tremendous number of pipes required, and we have been trying to cut installation costs by increasing the size of the pipes. All of our work is still in the experimental stage, but we have obtained good clearance on our mixed roaster and converter gases with a 3-ft. pipe treater 20 ft. long, and with 5 ft. velocity therein; and with a discharge electrode of a single No. 29 nichrome wire set in the middle of the 3-ft. pipe, with. a consequent electrode spacing of 18 in. The current used has been 150,000 to -160,000 volts, .and of course there have been troubles galore, relating particularly to insulation and rectifying. Blast-furnace gases did not give so good clearance, probably due to relative poverty in moisture and S03 content of blast gases to roaster-converter gases; making the blast gases the poorer in conductivity. Our experience has been so satisfactory that in our next experimental plant-built on a somewhat larger scale-we shall attempt a 4-ft. treater with greater electrode spacing, and a somewhat higher voltage-up to 220,000. As to fractional precipitation, mentioned by Mr. Howard, this idea was tried out at Anaconda last year (1913). Formerly our furnaces (Bruntons) roasting flue dust for the recovery of white arsenic, passed so great an, amount of dust to the settling kitchens that refining of this arsenical product was necessary to eliminate the 5 to 20 per cent. dust contained therein. Consequently the manufacture of As203 was effected in two stages, with a reverberatory roast of the first .product to obtain the final 99.5 per cent. As203. -

Jan 11, 1914

By J. B. Darby

In an investigation of various equiatomic alloys of transition elements, Dwightl did not find evidence for the CsC1-type ordered structure in VMn. More recently waterstrat2 has reported the occurrence of this structure in the alloy his sample had been homogenized at 1150°C and subsequently reannealed at 725°C after crushing to powder. The purpose of this note is to confirm the existence of the CsC1-type ordered structure in VMn and to report a lattice parameter. An equiatomic alloy was prepared by arc-melting under an argon atmosphere vanadium and electrolytic manganese having a purity of at least 99.9 pet. The composition was obtained by charging an excess of manganese and monitoring the weight loss until the stoichiometric composition was achieved; the assumption that the loss during melting was due to the vaporization of manganese appears to be a valid one.&apos; The calculated composition of the sample prepared was 49.85 at. pct V and 50.15 at. pct Mn. Specimens taken from the fractured as-cast buttons were wrapped in molybdenum foil and encapsulated in quartz capsules under vacuum; there was no evidence of a reaction between the alloy and foil. The X-ray patterns were obtained using filtered copper or chromium radiation with a Straumanis-type Debye-Scherrer camera having a diameter of 114.6 mm. The CrKa radiation is best suited for detecting the superlattice lines since it overcomes the slight difference in scattering powers of the components by making use of the anomalies in atomic scattering factor which occur when the frequency of the radiation is close to the characteristic absorption frequency of one of the elements.394 A specimen in the as-cast condition, as well as one which had been annealed for 1 week at 900°C and water-quenched, gave a diffraction pattern for the disordered bcc solid solution. However, when samples were homogenized at 900°C for 3 weeks followed by a subsequent anneal at 700°C for 6 to 7 weeks and then water-quenched or furnace-cooled, the (loo), (1111, and (210) Ka superlattice lines were observed in films taken with chromium radiation. An ao = 2.904 * 0.001 was determined by a Nelson-Riley extrapolation from a film taken with CuKa radiation. The author wishes to thank Mr. J. W. Downey and Mr. L. J. Norton for carrying out the experimental portion of this investigation. This work was performed at the Argonne National Laboratory under the auspices of the U.S. Atomic Energy Commission.

Jan 1, 1963

By Louis C. McCabe

The control of dusts and fumes of submicron size is involved in many process industries. This paper presents in tabular form the quantitative data from a number of metallurgical operations and discusses allowable discharge in terms of effluent-weight ratio. Typical installations for recovery of stack effluents are cited. THERE are many sources of smoke, fumes, gases, and dusts that may cause undesirable contamination in an industrial area. Fumes and gases are the result of chemical action or volatilization, while dusts are produced in processes of disintegration and dispersion. Commonly, smokes are suspended particles formed by combustion or destructive distillation. Methods for controlling smoke are generally known, and great improvements have been made in equipment for removing fine dusts and fumes from gases. In most of the industrial centers of the country, the chief duty of the air-pollution abatement agency is the elimination or reduction of emissions resulting from improper combustion. Correct methods of firing, proper fuel selection, and installation of properly designed equipment may accomplish this. It is becoming more widely recognized that much of the contamination of an industrial atmosphere is caused by dusts, fumes, and gases that are not related to the process of combustion. As such emissions are usually a functional part of plant operation, they rarely can be prevented even by better design and careful operation. When dusts, fumes, and gases are an integral part of the operation, mechanical equipment must be designed to remove these emissions. Most of the dusts and fumes that should be controlled are less than 1 micron in size. Control of such small particles is largely a new and untried field in many industrial areas. However, where conditions have been critical, effective control equipment for dusts, fumes, and gases has been in operation for many years. The problem is not one of smoke abatement and requires an entirely different set of standards for effective solution. Identical standards need not be applied to all industrial areas because of differences in meteorology, physiography, plant location, plant density, and nature of stack effluents. In this paper, discussion of control of atmospheric contamination by industrial plants refers specifically to the Los Angeles area, but the method of approach is applicable to any area where similar problems are encountered. Quantities of particulate matter reported in analysis of stack effluents indicate the need for standards of emission. Many types of dusts and fumes that contribute materially to the air-pollution problem are discharged into the atmosphere at a lower rate than 0.40 grain per cu ft at standard conditions. On the other hand, some stacks discharge at a higher

Jan 1, 1951

Discussion of the paper of L. A. DELANO, presented at the St. Louis meeting, October, 1917, and printed in Bulletin No. 129, September, 1917, pp. 1267 to 1286. L. A. DELANO.-Since this paper was written, our daily mill tonnage has increased, from 2100 tons to 2700 tons a clay. We now use 11,000 lb. of chrome-steel balls of 2 ½ -in. maximum diameter, for an average crushing capacity of 275 tons per 24 hr., this giving a much higher crushing efficiency. I wish to call attention to two typographical errors in my paper as published. On page 1271, Table 1, the screen analysis of ore at the Bonne Terre mill should be stated in inches instead of mesh. - On page 1272, "the rolls average 185 tons per 24 hr., and have shown by test that 250 tons per hour can be maintained" should, of course, read "250 tons per 24 hours." THE CHAIRMAN (0. M. BILHARZ, Miami, Okla.).-Is the increased mill capacity due to improvement in the re-crushing of middlings or to keeping middlings out of circulation and treating them separately? L. A. DELANO.-AS was shown in Mr. Rabling&apos;s paper (Bulletin No. 128, p. 1161) the tonnage was raised by about 400 tons by simply changing the arrangement of screen openings in the jig bed and using punched plate instead of woven-wire screen. Then, by adding a ball-mill, we are taking from the jigs a much larger tonnage of middlings than before or as much as the ball-mill will crush. By sending the ball-mill product to tables and flotation, the jig capacity for original ore is increased. CHAIRMAN BILHARZ.-In your opinion, the satisfactory operation of a Hancock jig on a given ore requires adjustment of the length of the different screens and careful selection of screen openings? L. A. DELANO.-I think it does. In order to decide what screen openings to use on the jigs, we did a great deal of experimental work, making screen analyses of the various hutch products, and then hand-sorting the galena, middlings and chat from each size screen to determine the percentage of galena in each. Then adjusting our jig screens, we gradually worked the process up to a very efficient basis. ERNEST GAYFORD, Salt Lake City, Utah.-I would like too ask Mr. Delano whether the work of the Allen cone has been quite as satisfactory as the manufacturers claim for it.

Jan 1, 1918

By Louis C. McCabe

The control of dusts and fumes of submicron size is involved in many process industries. This paper presents in tabular form the quantitative data from a number of metallurgical operations and discusses allowable discharge in terms of effluent-weight ratio. Typical installations for recovery of stack effluents are cited. THERE are many sources of smoke, fumes, gases, and dusts that may cause undesirable contamination in an industrial area. Fumes and gases are the result of chemical action or volatilization, while dusts are produced in processes of disintegration and dispersion. Commonly, smokes are suspended particles formed by combustion or destructive distillation. Methods for controlling smoke are generally known, and great improvements have been made in equipment for removing fine dusts and fumes from gases. In most of the industrial centers of the country, the chief duty of the air-pollution abatement agency is the elimination or reduction of emissions resulting from improper combustion. Correct methods of firing, proper fuel selection, and installation of properly designed equipment may accomplish this. It is becoming more widely recognized that much of the contamination of an industrial atmosphere is caused by dusts, fumes, and gases that are not related to the process of combustion. As such emissions are usually a functional part of plant operation, they rarely can be prevented even by better design and careful operation. When dusts, fumes, and gases are an integral part of the operation, mechanical equipment must be designed to remove these emissions. Most of the dusts and fumes that should be controlled are less than 1 micron in size. Control of such small particles is largely a new and untried field in many industrial areas. However, where conditions have been critical, effective control equipment for dusts, fumes, and gases has been in operation for many years. The problem is not one of smoke abatement and requires an entirely different set of standards for effective solution. Identical standards need not be applied to all industrial areas because of differences in meteorology, physiography, plant location, plant density, and nature of stack effluents. In this paper, discussion of control of atmospheric contamination by industrial plants refers specifically to the Los Angeles area, but the method of approach is applicable to any area where similar problems are encountered. Quantities of particulate matter reported in analysis of stack effluents indicate the need for standards of emission. Many types of dusts and fumes that contribute materially to the air-pollution problem are discharged into the atmosphere at a lower rate than 0.40 grain per cu ft at standard conditions. On the other hand, some stacks discharge at a higher

Jan 1, 1951

By R. A. Kinzie

THE major operating costs in a cement plant are labor, power, and fuel. The opportunities and methods of savings in labor and power parallel other industries. Because our industry&apos;s use of fuel is large and its method of use is unique, the devices adapted for saving fuel are of interest. In normal practice the raw material in the form of a dry powder or a mud is fed to a rotating inclined cylinder where it is dried, calcined, and clinkered. In a Lepol kiln the raw material is rolled up into little balls with water in the nodulizer, fed to a traveling grate on which it is dried and partially calcined and tben to a short kiln where the process is finished. The more usual methods of saving heat have been the use of long kilns with chains in wet process plants and the use of waste heat boilers in dry plants (fig. 1). At the Santa Cruz plant we have used a Lepol system kiln and achieved a fuel &apos;economy of 4.7 gal per bbl of clinker or about 704,-000 Btu per bbl. This can be compared with our old kilns using the same fuel and raw material which consume 7.8 gal per bbl or 1,130,000 Btu per bbl. These are gross Btu and not the net figures usually used in reports of foreign companies. Our average consumption for 1948 was 708,000 Btu per bbl of Lepol clinker, based on cement sold, and oil purchased. The overall fuel consumption for 1948 was 6.61 gal per bbl. The Lepol system consists of a nodulizer, a grate, and a kiln. There is the usual accessory equipment which is similar to that used in other cement plants. The following description covers the equipment in operation at our plant. The nodulizer is a cylinder 8 ft 10 in. in diam by 18 ft long set on a slope of 1/2 in. per ft, and rotated at about 10 rpm. It is driven by a 50 hp wound rotor motor drawing about 9 kw. The inside of the shell is cleaned by a continuously operating scraper which draws 0.1 kw. The dry raw material is fed to the nodulizer where, being sprayed with water, it rolls into small spheres about 90 pct being between 1/2 and 1 in. in diam and containing about 15 pct water. The nodules fall on the traveling grate where the hot gas from the kiln is pulled down through the

Jan 1, 1951

By R. A. Kinzie

THE major operating costs in a cement plant are labor, power, and fuel. The opportunities and methods of savings in labor and power parallel other industries. Because our industry&apos;s use of fuel is large and its method of use is unique, the devices adapted for saving fuel are of interest. In normal practice the raw material in the form of a dry powder or a mud is fed to a rotating inclined cylinder where it is dried, calcined, and clinkered. In a Lepol kiln the raw material is rolled up into little balls with water in the nodulizer, fed to a traveling grate on which it is dried and partially calcined and tben to a short kiln where the process is finished. The more usual methods of saving heat have been the use of long kilns with chains in wet process plants and the use of waste heat boilers in dry plants (fig. 1). At the Santa Cruz plant we have used a Lepol system kiln and achieved a fuel &apos;economy of 4.7 gal per bbl of clinker or about 704,-000 Btu per bbl. This can be compared with our old kilns using the same fuel and raw material which consume 7.8 gal per bbl or 1,130,000 Btu per bbl. These are gross Btu and not the net figures usually used in reports of foreign companies. Our average consumption for 1948 was 708,000 Btu per bbl of Lepol clinker, based on cement sold, and oil purchased. The overall fuel consumption for 1948 was 6.61 gal per bbl. The Lepol system consists of a nodulizer, a grate, and a kiln. There is the usual accessory equipment which is similar to that used in other cement plants. The following description covers the equipment in operation at our plant. The nodulizer is a cylinder 8 ft 10 in. in diam by 18 ft long set on a slope of 1/2 in. per ft, and rotated at about 10 rpm. It is driven by a 50 hp wound rotor motor drawing about 9 kw. The inside of the shell is cleaned by a continuously operating scraper which draws 0.1 kw. The dry raw material is fed to the nodulizer where, being sprayed with water, it rolls into small spheres about 90 pct being between 1/2 and 1 in. in diam and containing about 15 pct water. The nodules fall on the traveling grate where the hot gas from the kiln is pulled down through the

Jan 1, 1951

By L. C. Brown, C. St. John, C. C. Sanderson

The diffusion rate in Cu-Te couples is very sensitive to compressive stress, with a load of 20 psi making a significant difference to the width of the diffusion zone. At zero stress, two phases appear in the diffusion zone (Cu4Te3 and CuTe). Under compressive loading the third stable phase (Cuz Te) also appears, and its thickness increases progressively with increasing stress. The results are explained on the basis of an incipient Kirkendall porosity which restricts the transfer of atoms from the copper into the diffusion zone. DURING a study of the Kirkendall effect in Cu-Te couples prepared by clamping together the two components, it was found that the diffusion-zone width and shape in the plane of contact were not reproducible. Although the stresses involved in clamping are not normally sufficiently high to affect diffusion rates, preliminary tests established that the Cu-Te system is particularly stress-sensitive. The phase diagram for the system Cu-Te given in Hanssen1 shows that there is practically no solid solubility at either end of the phase diagram. Many areas of the diagram are not fully substantiated, but there appear to be three intermediate phases: Cu,Te—hexagonal in structure, having a grey luster; Cu4Te3—a tetragonal defect structure, having a red-purple luster; CuTe—orthorhombic in structure and having a golden-green luster. The existence of a fourth phase, the X phase at 37 at. pct Te, is considered doubtful. The composition ranges of the three stable phases are small, and are not accurately known. The phase diagram changes little with temperature up to 305°C, at which temperature a polymorphic transformation takes place in Cu2Te. The nature of the Cu-Te phase diagram indicates that the diffusion zone in a Cu-Te couple would consist of a series of layers of intermediate phases. The relative thickness of any one phase will depend on its diffusion coefficient and composition range.&apos; In this type of diffusion couple it is often found experimentally that some phases are not visible at all in the diffusion zone due either to a small diffusion coefficient or to a restricted composition range.3 Since the composition ranges of the phases in Cu-Te are not known, it is not possible to determine diffusion coefficients in this system from a knowledge of the phase thicknesses. Several investigations have been carried out to determine the effect of compressive stress on diffusion rates in multiphase systems. Diffusion couples of Ni-A1 have been investigated by Storchheim et al.4 and by Castleman and Seigle.5 Two phases (ß and ?) appear in the diffusion zone under zero stress and the thickness of both phases is progressively reduced with increasing stress. According to Storchheim et al.4 a stress of 25,000 psi reduces the thickness of the diffusion zone by 50 pct. In a-brass—?-brass couples the thickness of the 0 phase formed in the diffusion zone was reduced by 20 pct at a stress of 20,000 psi.6 In other investigations the compressive load has been observed to increase the width of the diffusion zone. In A1-U, several investigators3,8 have found the width of the whase UA13 to increase with stress. According to casileman,8 the rate of formation of UA13 at 520°C is 75 pct faster at a stress of 20,000 psi as compared with a stress of 2500 psi. In Cu-Sb the effect of stress is greater than in the other systems described. According to Heumann9,10 only one phase (y) appears in the diffusion zone at a stress of 500 psi, but at a stress of 850 psi two phases (y and k) are present. If a diffusion couple containing both y and k phases is annealed at a low stress level, the y phase grows at the expense of the k phase. EXPERIMENTAL The diffusion couples were prepared from electrolytic copper bar stock with a nominal purity of 99.92 pct and from tellurium of 99.7 pct purity. The tellurium proved difficult to machine because of its brittleness and a technique was developed for casting the tellurium into a graphite slab mold and spark-machining specimens from this slab. Both the copper and tellurium were produced in the form of discs 2 in. diam by approximately 1/4 in. thick with surfaces ground flat to 3/0 emery paper. The diffusion apparatus is shown in Fig. 1. Auni-axial compressive stress was applied to the system through a simple lever system. A stainless-steel rod actuated by the lever arm lay inside a stainless-steel tube. The diffusion couple lay on top of the steel rod, and pressure was applied to the couple between the rod and a plug welded into the center of the tube. To ensure a uniform stress across the couple, a hemispherical boss and cup were used to transmit the load to the diffusion couple. A 400-w tube furnace with a uniform hot zone 3 in. long slid around the stainless-steel tube and maintained the assembly at temperature. A thermocouple situated 3 in. from the specimen operated a proportional temperature controller which maintained the specimen temperature constant to ±2°C. Most diffusion runs were carried out at 250C although a few tests were made at other temperatures in the range 235° to 300°C. The specimens were inserted and removed with the furnace at operating temperature, and took only 2 min to reach diffusion temperature—a time small compared with the total diffusion time. All the diffusion experiments were carried out in a hydrogen atmosphere, since consistent results were obtained in hydrogen and nitrogen atmospheres and in

Jan 1, 1967

By J. D. Price, W. M. Bertholf

W. J. PARTON*—I have not had the opportunity to read this paper, and I do not have a written discussion. However, I thought it might be interesting for me to relate some of the experiences we had with equipment similar to the vibrating filter as described by the&apos; authors. At the Tamaqua flotation plant of the Lebigh Navigation Coal Co. approximately 40 tons per hour of froth concentrate carrying 60 pct by weight moisture are produced. The major problem encountered at this plant is the dewatering of this coal froth so that a satisfactory product can be sent to market. In the original design of the plant a centrifuge of solid bowl type was included for de-watering this material. The centrifuge did not work out as well as we had hoped. High maintenance costs and moisture content in the cake were obtained. A Robbins dewatering screen was installed at a later date with the idea of using it in conjunction with the centrifuge. The froth concentrate from the flotation cells was fed directly to the Robbins dewatering screen. The cake from the screen carried approximately 55 pct of the feed solids. Moisture in the cake was approximately 24 pct by weight. The underflow from the screen carried 45 pct of the feed tonnage at about 80 pct moisture by weight. The underflow product was then pumped into the centrifuge with the idea of using the cen-trifuge for recovering the tonnage lost through the screen. This circuit did not operate as satisfactorily as we expected. The only benefit derived was in the reduction in the power consumed by the centrifuge. The maintenance on the centrifuge was approximately the same as previously. The next step in our experiments was to pump the underflow from the screen into a cyclone thickener which was mounted directly over the vibrating screen. This thickener increased the concentration of the solids to approximately 60 pct by weight and dropped the mate- rial back 011 the filter cake which had formed toward the discharge end of the screen. Unfortunately, the screen was not capable of handling this additional tonnage, and our experiments stopped at that point. We have been considering installing a second screen to make possible the complete mechanical dewatering of this product by the use of the dewatering screen and the cyclone thickener. Another possibility under study is to pump the underflow from this screen to a thickener which is available in the flotation plant, and to combine this thickeued underflow with the original feed going to the screen. Again, however, a second dewatering screen will be required to handle the total tonnage. 0. R. LYONS*—I had an opportunity to read this paper ahead of the meeting, and I did a little pencil engineering on it. As Mr. Bertholf said, it is very difficult to make a comparison and to carry the results of work at one plant over to what might be expected at another. What I did was to find information on filtering operations more or less comparable to the type of operation that Mr. Bertholf has with his vibrating filter. The only information that I was able to find was for drum type filters, and I found the operating characteristics of the vibrating filter and the drum type filters were very similar. The moisture contents of the cakes were almost identical. The output per square foot was about the only way that I could compare their capacities— using square foot of screen area against square foot of filter area—and I found the capacity of the vibrating filter to be slightly greater per unit area than the capacity of the drum-type filters. W. H. NEWTON†—Do I understand that the only escape for the solids is by overflowing the thickener? That is, does the filter have a chance to recover all the solids except that lost in the thickener overflow ? W. M. BERTHOLF (authors&apos; reply)— Actually, the only escapc from that part of the circuit is over the top of the thickener. There are other places the fines could be lost in the washery. but once they get into that part of the circuit, they must go over the top to escape. W. H. NEWTON—I would like to ask Mr. Lyons if, in the study of rotary filters, he has any basis for comparison of operating costs? 0. R. LYONS—No, I had no information on costs. The only information I was able to find was on screen size, moisture content, and tonnage output per unit area. W. L. McMORRIS*—Are you wasting that overflow water or re-using it? W. M. BERTHOLF—Right now, we are not re-using it. D. R. MITCHELL† —What is the approximate per capita cost of one of these units? W. M. BERTHOLF—It appears to be somewhere in the neighborhood of $200, for the screen. W. H. NEWTON—The cost would be about $2500 for the complete unit including the vibrating power unit. G. A. VISSAC‡—I do not like to come on the floor after I have been talking so long, but I thought you might be interested in our experience in dewatering, as well as drying our very fine coals. We have used both centrifuge and vibrating screens. The type of vibrating screens we have used in Canada are called the Zimmer. That is a screen of German construction, and I guess it is along the same lines as the dewatering screens you are using now. We use wedge wires, and the minimum size opening is a quarter of a millimeter. In our experience, the cheapest way is still a dewatering bin. A dewatering bin takes 48 hr to do work that takes 20 min in a dewatering screen. We use old wedge wire from our driers which we cover with brattice cloth, and

Jan 1, 1950

By Jacques Steininger, Robert E. England

Single crystals of ZnTe and ZnTe1-,Sex with x up to 0.13 have been grown from the elements by temperature gradient solution zoning using excess tellurium as a solvent. Best results have been obtained with charges with the compositions 45/55 at. pct Zn, Te, for ZnTe and increasing amounts of selenium for ZnTe1-xSex. The temperature in the molten zone was maintained at about 1070°C with a gradient of about 10°C per cm. Chemical analyses of quenched ZnTe ingots show tellurium concentrations in the molten zone as high as 70 pct with concentration differences across the zone of 1 to 2 at. pct Dark dots which are observed by transmitted light microscopy in as-grown crystals can be removed by annealing in zinc vapor at 900 C. INTEREST in wide band gap semiconductors has led to a new study of ZnTe and ZnTel-xSex crystal growth. ZnTe is the only II-VI compound with a wide band gap (2.3 ev) that can be made p type with low resistivity. Attempts to make it n type with low enough resistivity to be useful for p-n junctions have so far been unsuccessful.1 ZnSe has a band gap of 2.65 ev but can be made n type only. However, ZnTel-xSex solid solutions with x as low as 0.36 have been made both highly n and p type2 with a minimum band gap around 2.12 ev3 at room temperature and appear to hold the best promise for efficient injection electroluminescence in the visible. ZnTe has the lowest melting point of the zinc chal-cogenides (1295°C) and consequently attempts have been made to grow crystals from both the liquid and the vapor phase.4 Complicated apparatus is required for growth from stoichiometric melts because of the high vapor pressures of the elements at the melting point of ZnTe and because of the problem of quartz devitrification. Small crystals have thus been grown in high-pressure equipment by Fischer5 and by Narita et a1.6 with pressures of the order of 50 atm of argon to prevent excessive evaporation from the melt. Large crystals of ZnTe can be obtained by growth from the vapor phase4 but they often present numerous dislocations and inclusions. An improvement in the quality of vapor- grown ZnTe crystals was reported by Albers and Aten7 by equilibration of mixtures of small crystals with compositions lying on either side of the solid single-phase field at fixed temperature. The same technique was later applied by Aten8 to the growth of ZnTe1-xSex crystals with less than 1 pct inhomo-geneity. Because of the higher liquidus temperatures of the solid solutions and the high vapor pressure of selenium, previous attempts to grow ZnTel-xSex from the melt have been limited and unsuccessful.9 The phase diagram of the Zn- Te system is reproduced in Fig. 1, based on data from Kobayashi10 and Kulwicki.11 Carides and Fishher12 have reported lower liquidus temperatures on the tellurium-rich side, but their data would require confirmation. The liquidus temperature on the tellurium-rich side decreases rapidly with increasing tellurium concentration and the Te2 vapor pressure over the liquidus also decreases accordingly.&apos;3 The decrease in liquidus temperature and vapor pressure therefore makes it possible to use conventional apparatus if there is a sufficient excess of tellurium in the melt. Single crystals of ZnTe have thus been grown by Kucza,14 in a modified Bridgman technique, from solutions containing up to 60 at. pct of Te by lowering unsupported quartz ampoules through a temperature gradient at about 1200°C. Under these conditions, the phase diagram indicates that the entire charge is initially molten. Crystal growth can therefore proceed by normal freezing and rejection of excess tellurium into the melt. The modified Bridgman technique has several major limitations. Because of the rejection of excess tellurium into the melt during freezing, the melt composition and the temperature at the growth interface vary continuously. They tend to follow the liquidus until the eutectic which is very close to pure tellurium (447°C, >99 pct Te). Since the solidus composition also varies with temperature,15 crystals grown by this method are inhomogeneous. They present small variations from stoichiometry which may affect their structure and physical properties. The simultaneous increase in tellurium content and decrease in melt temperature also combine to reduce the rate of diffusion of tellurium away from the growth interface, thereby causing constitutional supercooling and possibly dendritic growth. To minimize these effects, the initial melt composition is in practice kept relatively close to stoichiometry (less than 60 pct Te). This however limits the possibilities of operating at low temperatures and pressures. This paper describes a modified method of crystal growth by temperature gradient solution zoning (TGSZ) which is an adaptation of the temperature gradient zone-melting technique developed by pfann16 and of the traveling solvent method of Mlavsky and weinstein.I7 The TGSZ method now applied to the growth of ZnTe and ZnTel-xSex crystals is characterized by its very simple experimental arrangement and sample preparation technique. Unlike the modified Bridgman technique, there is no increase in the tellurium concentration in the melt and therefore it is possible to operate at lower temperatures and pressures. This method is also suitable for maintaining a constant temperature at the growth interface.

Jan 1, 1969

By H. H. Podgurski, J. C. M. Li, Y. T. Chou, F. N. Davis, R. A. Oriani

When an Fe-2 pct A1 alloy is nitrogemted at 500ºC with a gus tnixture (NH3-H2) in which the nitrogen activity has been kept Lou] enough to avoid the formation of iron nitride, a two-phase alloy is generuled which consists of AlN particles and a ferrite phase cotaining a heavy network of dislocations. The amount of nitrogen contained in such an alloy, when equilibrated with the nitrogenating atmosphere, far exceeds both that needed to satisfy the normal solution requirements of a Fe and that needed to convert all of the aluninuwi to AlN. This excess nitrogen is accounted for as being trapped on dislocations, adsorbed at the ferrite -AlN interface, and as an en-Iuznced lattice solubility in strained ferrite. This excessive uptake of nitrogen had previously been attribuled by other investigators to the formation of a nonstoichiornetric aluminum nitride. Isotope exchange experiments revealed various amomts of exchargeable N14 present in the originally nitrided samples that could not be removed by reduction with HS at 500ºC. This exchangeable nitrogen has been identified us that bound to the AlN -ferrite interface. Estimates of inter facial areas in alloys containing -3 pct by weight of A1N are as high as 10 sq m per g of alloy. ThE first1 of this series of papers described the experiments forming the basis for the elucidation of the mechanism of the formation of aluminum nitride particles within an Fe-A1 alloy. It was found that not only are dislocations necessary for the nucleation of the AlN particles but also the nitriding reaction in turn produces a dense network of dislocations in the ferrite matrix. It was also observed that nitrogen in excess of that needed for the formation of stoichiometric AIN is taken up by the alloy without the formation of an iron nitride. The present paper is an analysis of the excess nitrogen sorbed by the nitrided Fe-A1 alloy which considers the structure generated by the formation of the aluminum nitride particles. Because of the high density of dislocations, this system has proved to be quite useful in studying nitrogen-dislocation interactions. Wriedt and Darken2 have already reported such studies in a cold-worked ferritic steel. EXPERIMENTAL Nitrogen Sorption. The specimens of this alloy were cold worked (50 pct reduction) to 0.011 in. thickness and chemically cleaned in a 2:1 concentrated phosphoric acid-50 pct hydrogen peroxide solution before nitrogenation. The flowing nitrogenating atmosphere (11 pct NH3-89 pct H2) was established before the ni- trogenating temperature was reached. The same gravimetric and gas-flow equipment described in an earlier paper1 was also used in this investigation. Changes in nitrogen concentration were followed gravimetrically when establishing the isotherms. In the isotope exchange experiments, concentration changes were followed volumetrically. In some instances chemical analyses (Kjeldahl method) were used to check for material balances in both the gravimetric and volumetric procedures. Our objective was to obtain reversible nitrogen sorption isotherms for alloys equilibrated with NH3-H2 gas mixtures over a large range of nitrogen activity* and temperature. The *Defined as equal to PN H /P3/2 ,where P corresponds to partial pressure in atmospheres. Actually the nitrogen activity, aN, in the alloy equals K PNH3 /p3/2H2, where K is the equilibrium constant for the reaction NH3 = N + 3/2H2. upper limit for nitrogen activity was below that which would produce iron nitride; for reasons which will become apparent later, most of the sorption studies were made in the temperature range between 400" and 500&apos;C. The alloy sample studied most extensively in this investigation was given a series of successive reductions (100 pct H2) and nitrogenating treatments at 500°C to attain a stabilized structure. Presumably some dislocations were lost during these treatments. Throughout most of the sorption studies, temperature was held at ± 1°C and the gas-phase composition was held to k0.2 pet NH3. Based upon the results of numerous diffusion experiments with this alloy* the &apos;Results to be published in a third paper of this series. times chosen for equilibration were considered more than adequate, Nitrogen Isotope Exchange. The first exchange experiments were carried out by circulating a measured quantity of H2 and NH3* (with a predetermined isotopic *The NH3 was synthesized over a synthetic ammonia iron catalyst using H2, and N2, enriched with N15. AS the NH3 was formed it was removed continuously from the gas phase by circulating the mixture through a refrigerated (78ºK) trap. When most of the nitrogen had been converted to NH3, it was distilled from the trap into a glass storage vessel. composition, N15/N14) over a nitrided specimen at 450°C in a closed glass system. Attempts to reach the exchange limit isothermally, i.e., an isotopic ratio (N15/N14) in the gas phase identical with the extractable nitrogen in the nitrided alloy, were futile. The exchange rate between the gas phase and the alloy was too slow, involving many days. To circumvent the slow exchange with the gas phase, measured amounts of N15 and N14 were introduced into the alloy by nitrogenating with an NH3-H2, mixture at 500°C containing an N15/N14 ratio of 7.76; the charged specimens were then sealed by allowing an oxide film to form over them in air, and in this final condition the specimens were subjected to 500°C in vacuum for various times during which isotope exchange was allowed to proceed within the specimen. It was estab-

Jan 1, 1970