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By William E. Ford, Edward Salisbury Dana

5. Crystallography. - The subject of Crystallography includes the description of the characters of crystals in general; of the various forms of crystals and their division into classes and systems; of the methods of studying crystals, including the determination of the mathematical relations of their faces, and the measurement of the angles between them; finally, a description of compound or twin crystals, of irregularities in crystals, of crystal- line aggregates, and of pseudomorphous crystals. 6. Definition of a Crystal.- A crystal * is the regular polyhedral form, bounded by smooth surfaces, which is assumed by a chemical compound, under the action of its intermolecular forces, when passing, under suitable conditions, from the state of a liquid or gas to that of a solid. As expressed in the foregoing definition, a crystal is characterized, first, by its definite internal molecular structure, and, second, by its external form. A crystal is the normal form of a mineral species, as of all solid chemical com- pounds; but the conditions suitable for the formation of a crystal of ideal perfection in symmetry of form and smoothness of surface are never fully realized. Further, many species usually occur not in distinct crystals, but in massive form, and in some exceptional cases the definite molecular structure is absent. 7. Molecular Structure in General.- By definite molecular structure is meant the special arrangement which the physical units, called molecules, assume under the action of the forces exerted between them during the formation of the solid. Some remarks are given in a later article (p. 22 et seq.) in regard to the kinds of molecular arrangement theoretically possible, and their relation to the symmetry of the different systems and classes of crystals.

Jan 1, 1922

By HOWARD N. EAVENS

DURING the year just closed the bituminous industry has been marked by a continuation of the period of low prices and a steady deflation, accompanied by the closing of mines and the consolidation of small units into larger ones. This pro- gram has marked almost every field in the country, and it bids fair to continue for some time. Some figures recently published for Kentucky show that in 1924 there were 660 mines producing 45,147,000 tons; in 1928 the number had decreased to 537, while production had increased to 61,860,000 tons, and a similar movement is occurring all over the country. Prices throughout the early part of the year were very low, but during the fall and winter the prices received are more satisfactory than they were earlier in the year. One of the leading developments in the marketing of coal during the year was the trade practice movement, which began in the Harlan field, and has now been adopted in the Harlan, Hazard, Appalachian, Logan. Williamson and Kanawha fields. The purpose of this movement is to prevent the shipment of coal except on order, and by the publication of price lists to prevent much senseless price quotation. Where it has been practised the longest this movement has resulted in a considerable degree of stabilization, and, undoubtedly, it will help existing conditions very materially if it becomes universal.

Jan 1, 1930

By L. E. Shiffman

W. J. Parton—Those operators faced with the problem of treating fine coal whether in bituminous or anthracite will find this paper most timely. I would like to take this opportunity of discussing Mr. Schiffman's paper and at the same time express certain views relating to our Tamaqua plant. I would like to ask the author what type of impeller and diffuser is used in the Denver cells? Screen analysis of products from individual cells indicate that coarser material resists flotation and only floats after greater retention time in the last few cells. Also, the need for a scavenger screen to reclaim non-floated coal particles further stresses this point. I have always felt that more efficient means of cleaning coal between 10-mesh and 28-mesh existed than flotation. Reagent and power costs are high for the flotation process. When floating +28-mesh particles, cell capacity is lowered and some of the particles are lost with the refuse. The Tamaqua plant of the Lehigh Navigation Coal Co. floats —28-mesh coal and capacity of recoverable coal is 40 tph for 1800 cu ft of Denver cells; or 0.05 tons per cu ft of cell. At Kimberly 7.75 tph for 600 cu ft of cell gives 0.013 ton per cu ft of cell. At Bessie 14 tph for 800 cu ft of cell gives 0.017 tons per cu ft of cell. It would be appreciated if the author would comment on what he feels is the upper size limit of particle to attain most efficient utilization of the flotation process. The dewatering screw is a very interesting development since it offers a simple way to prepare coal sludge for more complete clewatering by drainage or mechanical dewatering on screen or filters. In other words it could be used to accomplish the same thing as a thickener tank. I would appreciate having the author's comment on how he thinks such a screw dewaterer would work on a froth.* The process as used in floating coal at the Bessie and Kimberly plants may be referred to as more of a bulk oil float in contrast to a froth flotation process. Experiments on increasing capacity of cells is most interesting since we are going through such an experi- mental period at the present time. Recently a double overflow was installed on our No. 30 Denver cells. So far results are not conclusive. In reviewing this paper the following comments are made pertaining to investigation of methods for increasing capacity: Supercharging: Supercharged air in matte flotation or for that matter the use of the normal amount of air drawn in by the impeller would in all probability cause such an aeration in the cell as to destroy the buoyant effect given to the coal particles by the excessive amount of kerosine used. In other words, air creates an agitation zone throughout the cell, creating a boiling and thereby giving a lower recovery in the cell. It would be interesting to know whether the 7 pct increase in recovery was with no air being admitted to the stand pipe. Changing Impeller Speed: The speed of a receded disc impeller for a No. 30 cell as recommended by the Denver Equipment Co. is, I believe, approximately 250 rpm. At this speed and using supercharged air in excess of 8-oz pressure, we have observed a boiling action in the cells. In our flotation we endeavor to obtain some degree of froth flotation using pine oil as a frother. The boiling action as caused by increasing the amount of air added to the cells is detrimental to recovery in froth flotation. It is our belief that to obtain increased recovery from a cell in froth flotation, additional air must be introduced but at the same time this air must be dispersed throughout the pulp in the form of small bubbles and this can only be done by increasing the speed of the impeller. Therefore, if Mr. Schiffman decreased the speed of the No. 30 impellers and at the same time continued to use supercharged air, the boiling action may have been increased because larger bubbles developed. The lower recovery as reported could be due to this factor. Decreasing the impeller speed will definitely decrease the power consumed but may have other disadvantages. First, we believe it will permit "sanding" in the cell and this in our opinion will increase the wear on the impeller and diffuser, especially so, if there is pyrite and/or sand present in the feed. "Sanding" in the cell when air is used, as in froth flotation, will effect the dispersion of this air and cause boiling.

Jan 1, 1951

By L. E. Shiffman

W. J. Parton—Those operators faced with the problem of treating fine coal whether in bituminous or anthracite will find this paper most timely. I would like to take this opportunity of discussing Mr. Schiffman's paper and at the same time express certain views relating to our Tamaqua plant. I would like to ask the author what type of impeller and diffuser is used in the Denver cells? Screen analysis of products from individual cells indicate that coarser material resists flotation and only floats after greater retention time in the last few cells. Also, the need for a scavenger screen to reclaim non-floated coal particles further stresses this point. I have always felt that more efficient means of cleaning coal between 10-mesh and 28-mesh existed than flotation. Reagent and power costs are high for the flotation process. When floating +28-mesh particles, cell capacity is lowered and some of the particles are lost with the refuse. The Tamaqua plant of the Lehigh Navigation Coal Co. floats —28-mesh coal and capacity of recoverable coal is 40 tph for 1800 cu ft of Denver cells; or 0.05 tons per cu ft of cell. At Kimberly 7.75 tph for 600 cu ft of cell gives 0.013 ton per cu ft of cell. At Bessie 14 tph for 800 cu ft of cell gives 0.017 tons per cu ft of cell. It would be appreciated if the author would comment on what he feels is the upper size limit of particle to attain most efficient utilization of the flotation process. The dewatering screw is a very interesting development since it offers a simple way to prepare coal sludge for more complete clewatering by drainage or mechanical dewatering on screen or filters. In other words it could be used to accomplish the same thing as a thickener tank. I would appreciate having the author's comment on how he thinks such a screw dewaterer would work on a froth.* The process as used in floating coal at the Bessie and Kimberly plants may be referred to as more of a bulk oil float in contrast to a froth flotation process. Experiments on increasing capacity of cells is most interesting since we are going through such an experi- mental period at the present time. Recently a double overflow was installed on our No. 30 Denver cells. So far results are not conclusive. In reviewing this paper the following comments are made pertaining to investigation of methods for increasing capacity: Supercharging: Supercharged air in matte flotation or for that matter the use of the normal amount of air drawn in by the impeller would in all probability cause such an aeration in the cell as to destroy the buoyant effect given to the coal particles by the excessive amount of kerosine used. In other words, air creates an agitation zone throughout the cell, creating a boiling and thereby giving a lower recovery in the cell. It would be interesting to know whether the 7 pct increase in recovery was with no air being admitted to the stand pipe. Changing Impeller Speed: The speed of a receded disc impeller for a No. 30 cell as recommended by the Denver Equipment Co. is, I believe, approximately 250 rpm. At this speed and using supercharged air in excess of 8-oz pressure, we have observed a boiling action in the cells. In our flotation we endeavor to obtain some degree of froth flotation using pine oil as a frother. The boiling action as caused by increasing the amount of air added to the cells is detrimental to recovery in froth flotation. It is our belief that to obtain increased recovery from a cell in froth flotation, additional air must be introduced but at the same time this air must be dispersed throughout the pulp in the form of small bubbles and this can only be done by increasing the speed of the impeller. Therefore, if Mr. Schiffman decreased the speed of the No. 30 impellers and at the same time continued to use supercharged air, the boiling action may have been increased because larger bubbles developed. The lower recovery as reported could be due to this factor. Decreasing the impeller speed will definitely decrease the power consumed but may have other disadvantages. First, we believe it will permit "sanding" in the cell and this in our opinion will increase the wear on the impeller and diffuser, especially so, if there is pyrite and/or sand present in the feed. "Sanding" in the cell when air is used, as in froth flotation, will effect the dispersion of this air and cause boiling.

Jan 1, 1951

By P. E. Fitzgerald

SOME readjustments in the research programs of most of the oil companics and petroleum engineering schools have been made necessary by the war. The most obvious change has been the conversion from production engineering to problems more closely related to the nation's was effort. Many laboratories now devote much of their time to studies on products to be derived from petroleum. such as synthetic rubber, toluene, and substitutes for critical materials. Others are working to improve motor fuels including high-octane gasoline and the special lubricants required by the wide geographical range of the present conflict. Of great importance is the experience of the geophysicists, who are now devoting a great percentage of their time on instrument research and production or special apparatus required by the armed forces.

Jan 1, 1943

By A. L. Bailey, B. A. Landry

W. W. ANDERSON and G. E. KELLER*—We want to compliment the authors on this very thorough paper. It gives information which the coal industry has needed for some time. We hope that the additional information which the authors are collecting will he available shortly. The mixing and riffling procedure that was followed for experimental purposes is obviously not practical in routine float-and-sink testing because of the particle size degradation which would result in handling the sample so many times. It is important to obtain our tloat-and-sink fractions with a minimum amount of handling of material. A statement is made in the paper (p. 80) that "the variable most likely to affect the size of sample required to meet a given preassigned accuracy would be the state or degree of mixing of the coal." We agree that this is a large factor, but do not believe it is the most important factor. Our own opinion is that the most important single factor governing the total gross weight of sample that must be collected is the percentage of the weight of material in the smallest fraction that results from the screening and float-and-\ink operations. In other words, size of sample is governed by the total number of fractionations that must he made, and the distribution of material within the fractions. We can imagine a coal with perfect mixing, but with such a small amount of material in some float-and-sink fraction in one of the coarse sizes that a much larger sample would have to be taken than would be the case with very poorly mixed material, but with a large percentage of coarse material more evenly distributed in all float-and-sink fractions. Our own observation of many float-and-sink tests that we have run in our own organization on many types of coal is that the size of sample that must be used on fine size float and sink is governed more by the requirements for weight of material to be used for analysis in the laboratory than by weight of material necessary to obtain accurate float and sink percentage of weight values. In other words, it is our opinion that very small samples can be used for float-and-sink fractionation in the fine sizes, but that accurate analysis of the fractions will depend on a larger weight of sample being pulverized for the laboratory than is necessary to establish the float-and-sink distribution with respect to weight. A. L. BAILEY and B. A. LANDRY (authors' reply)—The authors thank Messrs. Anderson and Keller for their comments based on long experience. It is agreed that the involved mixing and riming technique used may be disadvantageous from the standpoint of degradation. Fortunately, the paper does point out that the extended riming was unrewarding in causing further mixing. Two large unknowns remain, however: (1) how much of the mixing from the presumed highly unmixed state in the bed was achieved toward the random state during blasting, loading, transportation, screening, and further transportation to the point where the gross sample was taken, and (2) how much of the mixing took place during the preparation described preceding riming. As has been pointed out by one of the authors.6 the degree of mixing has a very large effect on the size of sample required and there are still too few experimental data to show at what stage of coal handling most of the mixing occurs. The discussion states that the weight of material in a screened fraction, or in a float-and-sink fraction, is more important than the mixing factor. We do not believe that these factors are comparable in this instance inasmuch as our purpose was to give minimum sampling requirements to achieve a preassigned accuracy in the percentages of float, middlings, or sink, and nothing more. The gross sample had already been screened and no further division by screening was made or contemplated; also, it was not intended that the middlings and sink fractions would necessarily be adequate for percentage ash or other determination. In other words, the sample obtained by the method outlined is not intended for washability studies but only for preparation plant control. Further experimental work has been done, since the paper was prepared, to investigate the effect of increasingly larger top and bottom sizes on the variability of float, etc., of a double-screened coal from Western Pennsylvania. Results will be published and eventually attention is to be given to the preparation of sampling specifications. E. H. M. BADGER*—I should like the authors to explain more fully the fundamental assumptions on which their Eq 4 is based. The equation is of the form s2 = p(l - p) which is the usual expression for the (standard deviation)2 when the chance of finding a particular kind of particle in the sample is proportional to the number fraetion, p. But instead of the number fraction, the authors have used the weight fraction, WF/W. The chance of finding a particular kind of particle in the sample can only be proportional to the weight fraction, if the average ?eig?ts of all kinds of particles, that is, float, midlings, or sink, are the same. Surely a much more justifiable assumption would be that the average volumes of the particles are the same, and, if this is so, Eq 4 would not be true. This may be demonstrated as follows: Let be the weight fraction of float, middlings, or sink, dl the density of this fraction, and d2 the density of the rest of the coal. Then assuming that the average volumes of the pieces in the three classes are the same, the number fraction, p, is given by ? P = d1/l-?/d2 + ?/d1 = ?d2/d1 + ?(d2-d1) The weight fraction, w, in terms of p is given by ? = pd1/(l-p)d2 + pd1 = pd1/d2 + p(d1-d2) _____ [61

Jan 1, 1950

By AIME AIME

T HE Mining Methods Committee held its initial meeting* on Tuesday afternoon, with F. W. Bradley in the chair and W. Y. Westervelt as vice- chairman. The first paper to be presented was "A Plea for a U. S. Court of Patent Appeals," for which Kenneth W. Greenawalt ably pleaded. The paper (which was published in full in last month's issue) is so carefully prepared that no synopsis can do it justice. It discusses the opposed views of some patent lawyers and other lawyers and members of the judiciary as, for example, Chief Justice Taft who is quoted as saying in 1921: "I think it is a great deal better to take a first class lawyer and a first-class judge and make him a good patent expert than it is to take a patent expert and try to make him a first-class lawyer and a good judge." Mr. Greenawalt argued the need for specialized scientific and engineering interest and understanding to enable a lawyer or judge to prepare or interpret patent specifications and decide the originality necessary for a valid invention. He proposed the special U. S. Court of Patent Appeals to also counteract the costly confusion and injustice now ruling where a patent may be declared valid in the courts of certain States and invalid by the courts of other States.

Jan 1, 1930

By Mark C. Malamphy

AT present the Federal Government represents the only organization applying geophysical methods of prospecting in Brazil. The geophysical work of the National Department of Mineral Production, which will be described in the following pages, must be considered as a program of experimental work designed to demonstrate the applicability of the more or less "standard" methods of geophysical prospecting to various problems of economic interest in Brazil by means of practical examples of results obtained in certain typical areas. Our work is somewhat similar to that of the Imperial Geophysical Experimental Survey of Australia, but our task has been greatly simplified by the ever increasing number of technical publications relative to the theory of instruments and methods.

Jan 1, 1936

By T. P. Chen, F. W. Bowdish

Studies made with a captive bubble apparatus on the sulfidization and collection by amyl xanthate of true chrysocolla specimens have defined the ranges of pH value and sulfide concentration which permit contact between the bubble and the mineral surface. Titanium compounds were the most effective of the materials found to activate the sulfidization of chrysocolla. With titanium activation, the contact angles and the ranges of pH value and sulfide wncentration giving bubble contact were all increased. Chrysocolla ores were concentrated by flotation. Chrysocolla ores occur at many localities in grade and quantity sufficient to make mining and millin feasible, but no satisfactory method of concentratio has been found. Although chrysocolla may be leached with acid, only those ores without acid-consuming gangue may be leached economically. Because of its potential importance, a study of the conditions nece sary for flotation of chrysocolla has been carried ou The literature contains a few references to flotation of chrysocolla. Two methods were developed by the U. S. Bureau of Mines.1,2 The first consisted of a fatty acid soap and a high xanthate as collectors of chrysocolla from a synthetic ore, while the second involved the use of hydrogen sulfide and xanthate. Ludt and DeWitt3 demonstrated the difference in adsorptive powers of chrysocolla and quartz for bas triphenyl methane dyes and suggested the use of butyl, hexyl or octyl-substituted malachite green as collector. Jackel4 emphasized the effects of combin tions of reagents such as Aerofloat 31, pine oil, and Reagents 404 and 425 with sodium sulfide and zinc hydrosulfite as conditioning agents. Although he reported recoveries of 89% from a synthetic ore and 98% from a natural ore containing azurite, malachite, chalcopyrite and chrysocolla, careful application of Jackel's method to chrysocolla from Tyrone, N.M., failed to give a high recovery. MATERIALS AND TECHNIQUE Samples from Inspiration, Ariz., and Tyrone and Magdalena, N. M., were used for experimentation and verified as true chrysocolla by leaching tests, specific gravity tests and X-ray diffraction. Chrysocolla does not dissolve at pH 4, although malachite and azurite do. Chrysocolla is about half as dense as the copper carbonates. X-ray diffraction analyses by the powder camera method confirmed the samples as true chrysocolla. A captive bubble apparatus, which cast an enlarged image of the air bubble and the mineral surface upon a screen, was used to check on the character of the surfaces. The specimens were prepared by grinding a flat surface on a glass plate using fine abrasive; then they were washed and kept in distilled water until they were to be treated with reagents. Before each reagent treatment, the specimen was carefully checked for cleanliness in the captive bubble apparatus. It was assumed that the surface was clean if, after fine grinding and washing of the specimen, the bubble would not stick. Specimens were handled with glass forceps, and precautions were taken to avoid contamination of the mineral surfaces. Contact angle measurements were carefully made several times on each treated specimen to obtain reliable average values. EFFECT OF pH VALUE AND SODIUM SULFIDE CONCENTRATION In each experiment, a specimen with a freshly ground surface was immersed for 10 min in a solution of sodium sulfide, washed and immersed for 15 min in a solution containing 30 mg per 1 of potassium amyl xanthate. The specimen was then washed again in distilled water and tested for contact angle in the captive bubble apparatus while submerged in distilled water. In this series of experiments, the pH of the sulfidizing solution was varied from 3 to 7, and the concentration of sodium sulfide, containing 60% Na2S, was varied from 50 to 650 mg per 1. Many combinations of pH value and sulfide concentration resulted in no contact between the bubble and the surface, but over a limited range of conditions, contact angles varying from 24ºto 52ºwere obtained. The data in Fig. 1 show sulfidization conditions that lead to bubble contact and those that do not. The region of contact is surprisingly small, which may indicate why flotation of chrysocolla involving sulfidization has proven so difficult in practice. Several features of the system are illustrated in Fig. 1. In the region between pH values of 4 and 6 with sodium sulfide concentrations below about 350

Jan 1, 1963

By G. Purcell, S. C. Sun

In an attempt to determine the relative collecting ability of 18-carbon fatty acids, studies were performed on rutile in aqueous solutions of the fatty acid soaps. The preceding article reported the electro-kinetic properties; this article outlines the flotation behavior. Results of these flotation experiments are described and correlated with the electrokinetic results. Recent studies of the electrokinetic1-4 and the electrochemical5,6 properties of a few solid-liquid interfaces have provided a better understanding of the flotation process. A number of investigators have attempted to determine the relative collecting ability of 18-carbon fatty acids, but their published results (even for the same mineral) vary widely. Such lack of agreement indicated a need for further investigation. In an effort, therefore, to resolve the problem, electro-kinetic studies were made on rutile in aqueous solutions of the fatty acid soaps. Following the determination of the electrokinetic properties, the flotation behavior of rutile was studied. Results of these flotation experiments are described in this paper and are correlated with the electrokinetic results. MATERIALS AND EXPERIMENTAL PROCEDURE Materials: Pure -28, + 35-mesh rutile crystals were used for all flotation tests, and nitrogen-saturated conductivity water was used throughout. Sodium hydroxide and hydrochloric acid were added for pH regulation. The methods of purification for these materials and the preparation of the soaps have been described elsewhere. 7 Equipment: A Hallimond cell, constructed in a manner similar to that described by Fuerstenau, Metzger and Seele,8 was used for the flotation of mineral particles; however, a coarse pyrex frit was substituted for the capillary. Procedure: Purified nitrogen was led through a two- way stopcock into a graduated cylinder partly filled with water. The gas forced water from the cylinder back into a header tank until the water level in the cylinder coincided with a predetermined mark. Reversal of the stopcock then allowed water in the tank to force nitrogen into the cell until the water in the graduated cylinder rose to a second predetermined mark. In this way a constant volume of nitrogen under practically constant pressure was used for each flotation test. However, the flotation time varied, depending upon the amount of mineral floated and the pH of the solution. Rutile crystals were transferred under water from a storage bottle by a glass scoop holding 1.7 g. Consistency of the scoop samples was good, varying from a low value of 1.67 to a high of 1.74 g. The water added to the conditioning bottle during mineral transfer was drained off, and then 2 cu cm of either hydrochloric acid or sodium hydroxide were added. The concentration of pH regulator was adjusted to give approximately the final soap solution pH that was required. The order of addition of reagents did not affect the results within the limits of experimental error. Soap solution of the required concentration was added under nitrogen pressure to fill the bottles completely. Conditioning for 1 hr was carried out on rolls rotating at 35 rpm. After conditioning, 2.5 cu cm of solution were run off into the container of a Beckman (model G) glass electrode pH meter. The electrodes were rinsed in this solution, which was then discarded, and 2.5 cu cm more were added for pH determination. The remaining solution and the mineral were transferred to the cell; care was taken to ensure that all mineral was washed out of the bottle by the conditioning solution. With the cell back in its flotation position the liquid just reached the desired level, and the test was started immediately. The amount of agitation in the cell was kept constant, and flotation was carried out without the use of a frother. In each series of ten tests one was run with no collector added to ensure that the mineral had not become contaminated, and two were conditioned at the same pH to check reproducibility. After each test the cell was dismounted, soaked in cleaning solution, washed in hot water and then rinsed with distilled water.

Jan 1, 1963

By JOHN R. SUMAN

IT appears now that the conflict with the totalitarian states will be a long-drawn-out struggle. The course of this war up to now indicates that this may well be the first major conflict where man power has not been the vital and determining factor. Mechanized warfare has made it possible for relatively small, well-equipped groups to outmaneuver and defeat large armies which lack the necessary modern equipment. Under these circumstances, ultimate victory becomes a matter of resources and productive ability. The important question is not how many soldiers can he put into the field, but the volume and speed in producing the armaments essential to ensure a victory. The resources available to the opposing nations and the efficiency of their systems of enterprise and production will be primary factors in determining the ultimate outcome. Germany had a head start of eight years in the armament race, and it is not easy to overcome such an advantage overnight.

Jan 1, 1942

By R. C. Gifkins, K. U. Snowden

The value of the index n in power ktivs for the stress sensitivity of minimum creep rale at lead is derived front results drawn from lite literature and from previously unpublished nork on commercial (99.99 pel) and high-purity (99.999 pel) lead polycryslalline and hi crystal specimens. In tests al 0.5Tm (22 to 50'C) for slvesses below 250 psi, n fulls to mily for poly-cr,yslullirle specimens, single crystals, and bicrystals, and toy grain boundary sliding in bicrystals. Between 250 and 500 psi there is a tyansilion range and, for the polycrystalline specimens al least, u high-stress regime for 500 to 1500 psi where n is 5 or 6. These results are such that none of the suggested stress taws can he used to extrapolate to very loir stresses. Meclianisms for deformation in Ike grains and toy grain boundary sliding in the low-strcss regime are outlined. In particular, the mechanism for grain boundary sliding involves sliding controlled by diffusion from tensile to compressire Ledges. predictions based on this model give promising numerical agree-nicul with experiment. II is suggested that the mechanism for grain boundary sliding may he important in other circumstances, e.g., in creep of ceramic materials or superplaslicity, because it can operate with lille or no dislocation aclirity. WhEN the stress dependence of secondary creep rate is represented by a power law the values taken by the stress exponent n are found to vary between 1 and 7, see, c.g., Garofalo.' In Eq. 1 11 u is the applied stress and A a constant. The case for accepting values of v = 1 rests principally upon tests at high temperatures (>0.9Tm) and there have only been isolated tests at lower temperatures (rather than plots of creep rate against stress) for which the creep rates are such that some form of Nabarro-Herring creep with n = 1 is applicable. Hanson5 and Greenwood and cole6 plotted creep rate against stress for tests made in the vicinity of 0.5Tw, and found a "creep yield", so that below a certain low stress the creep rate was linearly related to stress: these observations appear to have been subsequently ignored. Various models have been proposed which agree with a large body of experimental results in which n equals -5 at high stresses (e.g., weertman7 and McLean8). Various alternatives to Eq. [1] have been proposed principally as a means of unifying creep data, but sometimes, it seems, in order to obviate the necessity for assuming a series of regimes of deformation associated with the various values of n; further refer- ence to these will be made in the section on stress laws. This paper calls attention to extensive results which show n = 1 for the creep of lead at room temperature (0.5 T,). RESULTS Fig. 1 is a composite diagram based on figures in the literature6,9,10 with additional results obtained by the present authors and their colleagues11,12 in the course of a number of investigations not directly concerned with stress sensitivity. In Fig. 1 In creep rate is plotted against In stress. The curves show results for two kinds of material. Lead I is of commercial purity (99.99 pct Pb) and lead IT a specially refined material, hydrogen-purified to remove oxygen; it contains 99.999 pct Pb. Curve A is for lead I in polycrystalline form (grain diameter 0.02 to 0.05 cm) at room temperature (22' to 26°C). Curve B1 is for lead I, polycrystalline, tested at 50C. Curve B2 is for lead 11, polycrystalline (grain diameter 0.02 cm), tested at room temperature (22 O- Curves C to F relate to tests made of bicrystals of lead 11: all of the same nominal orientation ("Y" in Ref. 12). Curves C and V are for creep within the component crystals of the bi crystals at 22°C (AB and CD in Fig. 2). Curve E is for creep measured in a gage straddling the boundary, approximately 0.15 mm either side (BC in Fig. 2). Curve F shows rates of grain boundary sliding (as distinct from strain rates in the other curves), obtained by averaging the offsets of six marker lines on the bi-crystal boundaries. The principal feature of the results is that the stress sensitivity falls into two distinct regimes, according to whether the stress is below approximately 250 or above 500 psi (there is a transitional range between 250 and 500 psi). The new result is that below -250 psi two of the curves (A and BI) give a value of n 1, and the other curves also drop below n - 2 to -1.5 but do not extend to low enough stresses to show clear evidence of n 1. At very high stresses the curves tend to give values of n - 6, as previously determined in other investigations. Curve R2 for the high-purity lead in polycrystalline form at room tenlperature almost merges with B, and thus gives new significance to the values for stresses of 150 and 200 psi; previously'3 these points had seemed to fall away from the curve of slope -3, but they now can be seen as almost completing a transition to n = 1. It should be noted that there was originally considerable apparent scatter in the results for the high-purity lead. However, this was found to be associated with annealing conditions or variations in residual content of oxygen and curve B2 was constructed using the highest rate (i .e., the rate for the purest lead) determined for each stress during the course of various investigations over the years: altogether, some forty tests were used in constructing curve R2.

Jan 1, 1968

By H. E. Criner, M. G. Driessen

Maurice Rey—The influence of cyclone diameter upon the fineness of separation is an important point which, however, cannot be discussed adequately if the injection pressure or the rate of flow are not specified. Perhaps some light can be thrown on the matter by using the formulas derived by Dahlstrom. Let us consider several geometrically similar cyclones where the apertures e and b are equal and proportional to the diameter D and which are operated with the same pressure drop. Eq 8 of Dahlstrom's paper can be written: Q Q = K D'. " or. if F is constant: Q = K D18 K is a constant of proportionality. Introducing this value of Q in eq 13 gives elimination efficiency = K D ,41 Elimination efficiency, in the terminology of Dahl-strom, means the diameter of particles, in microns, which divide equally between the underflow and the overflow. This denomination is regrettable and it would be preferable to call it diameter of separation or characteristic size or any other name connoting a size rather than an efficiency. Whatever the name used, the above equation shows a slow increase in the fineness of separation when the diameter of the cyclone decreases. For example, if a 14-in. cyclone gives a 400-mesh separation (37 microns), geometrically similar cyclones, having the same pressure drop will give separations at the sizes shown below.

Jan 1, 1951

By M. G. Driessen, H. E. Criner

Maurice Rey—The influence of cyclone diameter upon the fineness of separation is an important point which, however, cannot be discussed adequately if the injection pressure or the rate of flow are not specified. Perhaps some light can be thrown on the matter by using the formulas derived by Dahlstrom. Let us consider several geometrically similar cyclones where the apertures e and b are equal and proportional to the diameter D and which are operated with the same pressure drop. Eq 8 of Dahlstrom's paper can be written: Q Q = K D'. " or. if F is constant: Q = K D18 K is a constant of proportionality. Introducing this value of Q in eq 13 gives elimination efficiency = K D ,41 Elimination efficiency, in the terminology of Dahl-strom, means the diameter of particles, in microns, which divide equally between the underflow and the overflow. This denomination is regrettable and it would be preferable to call it diameter of separation or characteristic size or any other name connoting a size rather than an efficiency. Whatever the name used, the above equation shows a slow increase in the fineness of separation when the diameter of the cyclone decreases. For example, if a 14-in. cyclone gives a 400-mesh separation (37 microns), geometrically similar cyclones, having the same pressure drop will give separations at the sizes shown below.

Jan 1, 1951

By S. A. Bradford

Internal-oxide precipitates in decarburized a iron alloys were studied by microscopic and X-ray methods. Diffusion of oxygen is primarily trans-granular, although large amounts of manganese or PhosPhorus cause preferred grain boundary dimsion at temperatures below 1450OF. Transgvanular internal oxidation follows the parabolic rate law with an apparent activation energy of 60 kcal per g-atom for decarburized rimmed steel and around 50 kcal per g-atom for higher alloy contents. The internal oxide is (Fe,Mn)0. Evidence was found for a miscibility gap in the FeO-MnO system. UNTIL very recently, the internal oxidation of metals was studied primarily as a scientific curiosity or, in a few cases, as a means of strengthening alloys by precipitation hardening. However, with the recent development of low-carbon enameling sheet steel, internal oxidation has become a problem of practical importance to the steel industry. For example, in 1961 it was reported1 that internal oxidation of steel can occur during decar-burization by open-coil annealing and will reduce the notch ductility of the sheet unless the process is carefully controlled. The present study was therefore undertaken to learn more about the rates and mechanism of oxygen diffusion and oxide formation in iron alloys. BACKGROUND The process of internal oxidation has been well-defined in the literature:',' oxygen dissolves in an alloy, diffuses inward from the surface of the metal, and reacts to form a precipitate with the alloying element that will provide the most stable oxide. he growth of the finely divided so-called subscale, i.e., the internal-oxidation zone, depends on the diffusion rates of both the oxygen and the reactive element.4 Investigators have generally found that increasing the temperature increases the size of the oxide particles, the rate of subscale growth, and the tendency to transgranular diffusion. With very few exceptions, the square of the thickness of the internal oxide layer is directly proportional to the reaction time. Given two conditions easily satisfied for iron systems— a) an oxygen solubility much less than the concentration of the alloying metal and b) an oxygen-diffusion rate to the oxide boundary much faster than that of the alloying element—then the general expression developed by Rhines and co-workers5 for the parabolic growth rate of the internal-oxide zone can be simplified to the following form: where Co and CM are, respectively, the solubility of oxygen and the concentration of the alloying element, DO is the diffusion coefficient of oxygen, O/M is the weight ratio of oxygen to metal in the precipitated oxide, and x is the thickness of the internal-oxide zone after an annealing time t. Both the oxygen solubility and diffusion coefficient can be approximately expressed as functions of temperature by Arrhenius-type equations: in which H and Q are, respectively, the heat of solution and the activation energy of diffusion. Consequently, the apparent activation energies calculated from Arrhenius plots are the sum of the heat of solution of oxygen in iron and the activation energy for diffusion of oxygen. The data, if not the interpretation, of Schenck et al.8 bear out the fact that oxygen diffuses in the atomic form. The general rate law for atomic diffusion is: the reaction rate being proportional to the square root of the pressure at low pressures. Benard and Moreau8 studied both the surface oxidation of Fe-Ni alloys and the gradual penetration of oxygen into the metal. They observed that oxide particles first form along grain boundaries and then grow to form continuous films that eventually envelop the grains. The parabolic rate law does not usually apply in these cases, especially at the higher temperatures. The oxide formed is wustite which gradually transforms into Fe3O4 and finally into Kennedy and coauthors8 examined Fe-Ni alloys with 26, 75, and 84 pct Ni oxidized at 800°C and

Jan 1, 1964

By Pual M. Tyler

BLIZKRIEG tactics in the present war have consumed metals on such a profligate scale that some of the best-laid procurement plans for civilian and military needs of even a year ago seem in retrospect incredibly meager. Conservation of raw materials has reached an all-time climax in Germany, where metals are worth more than human life and throwing away an empty toothpaste tube may be legally punished by death. Even the United States and the British Empire, proud masters of nine tenths of the world?s known mineral reserves and processing plants, are being driven to metals and feverishly expanding production facilities that not long ago were deemed overbuilt. After the war is over and inevitable postwar readjustments are completed, it is reasonable to expect that purchasing power ? or at least the ability to procure the comforts and luxuries of life ? will be distributed among vastly larger population than ever before, accelerating the rising trend in demand for industrial raw materials in ever greater quantity and variety.

Jan 1, 1942

By G. R. Love, M. L. Picklesirner

THE use of color adds a new beauty, power, and versatility to metallography. This has been amply demonstrated in a number of public exhibits and on the walls of corporate, government, and university metallographic laboratories around the world. Indeed, in a number of cases, the color not only is of esthetic value but is scientifically essential to the competent examination of particular samples and systems. Optical strain analysis,' determination of true grain size in U-A1 alloys: phase identification in Nb-base alloys,3 analysis of transformation rates in heat-treated Nb-Zr alloys,4 measurement of solidification segregation in cast Nb-Zr alloys,' study of the intermediate phases in Nb/Sn diffusion couples,6 investigation of the oxidation kinetics at various surface orientations in single crystals,7'8 and a number of other research efforts9'10 would have been vastly more difficult without the extra clarity and distinction introduced by color—either the colors resulting from particular polarized light techniques or the interference colors obtained by oxidation. It is unfortunate that the beauty of colored micro-structures cannot be shared more widely, but the economics of publishing a technical magazine apparently prohibits color plates except under extraordinary circumstances. It is doubly unfortunate that no convenient, general method exists for communicating the information available in colored microstructures to the scientific community. True, in some instances the color changes observed are dramatic enough that direct black and white photography is adequate. In photoelastic stress analysis, several orders of interference fringes may be produced and it is frequently desirable to suppress the color effects (use monochromatic light) to simplify interpretation. On the other hand, relatively minute color variations may be readily detectable by eye, be of considerable assistance in interpreting a structure, and yet be enormously difficult to reduce to an unambiguous black and white print. In order to illustrate a possible compromise or solution to the above problems, we wish to show three black and white photographs of the same region of an Nb/Sn diffusion couple whose interpretation depends heavily upon use of color techniques. These micro-structures were obtained from a section through a rod consisting of commercial-purity niobium tubing filled with 99.995 pct Sn (melt-filled in 10"6 Torr vacuum). The composite rod, measuring 500 mm long, was bent into a hairpin shape and inserted into water-cooled copper grips in a vacuum high-temperature furnace. The rod was outgassed for 2 hr at a furnace temperature of 800°C and was further heated by self-resistance using a 2.2-kva ac power supply. The rod was raised to 1910°C over a 4+-hr period, held for 15 min, slow-cooled to 1500°C over a -hr period, and free-cooled to room temperature (all temperatures were measured with W5Re/W26Re thermocouple). Throughout the heat treatment the ambient pressure was kept below 8 x lo-' Torr. Metallographic preparation of the sample was completely conventional except that it was necessary to extend the grinding steps to remove damage in the brittle NbsSn phase introduced by sectioning. No satisfactory chemical or electrochemical etch has been found for these diffusion couples; of those which have been tried, any that attack the niobium-rich phases at all attack the tin-rich phases disastrously. However, the final polishing steps did produce a slight relief effect and this, coupled with anodizing, yielded excellent clarity in the microstructures for direct observation. The anodizing voltage was chosen to give maximum change in color per unit change in composition. In this case, indeed normally, this maximum sensitivity occurred in the blue-to-red color range. The pure niobium tube wall anodized to a relatively bright blue

Jan 1, 1967

By AIME AIME

A FALL meeting that should have repercussions both in the "Transactions" and MINING AND METALLURGY was that of the Industrial Minerals Division (Nonmetallics) at Wilmington, Oct. 21-23; headquarters, Du Pont Hotel. The sixteen technical papers and two addresses were substantial and interesting. Moreover, in every instance but one, the author made the presentation, and the one exception must have been next of kin because the ensuing discussion indicated his command of the subject. The meeting schedule clicked at every turn, thanks to Dr. Gillson, chairman of the local committee, and even the four field trips adhered to the time table. The program pre-empted morning, noon, afternoon and night two general luncheons, two dinners, and an evening technical session reminding one of the Annual Meeting. Only the registration was disappointing - about 80.

Jan 1, 1943

By M. J. Pool, P. J. Spencer, R. V. Miner

The partial molar heat of solution of rhodiunz in liquid lin and Rh-Sn alloys has been measured as a function of rhodium concentration at 700" , 725" , 750" , and 775°K. The values at infinite dilution are very exo thermic, ranging from -29,950 to -28,260 cal per g-atom Rh at 700" and 775"K, respectively. At the solubility limit the heat of solution becomes sharply nzore exothermic and has permitted the liquidus boundary to be accurately established at each temperature. From the measurements in the two-phase region of liquid Plus RhSn, the heat of formation of RhSn,has been determined. A large increase in the heat of formation between 725" and 750°K suggests the possibility of a phase transformation in this compound. V ERY few measurements have been made of the heats of solution of transition metals in liquid tin; yet those values that are available are of great interest because of their very large exothermic nature. For example, the heat of solution at infinite dilution of palladium in tin has been measured as about -26,000 cal per g-atom (625" to 800°~),' while the heat of solution at infinite dilution of platinum is even more exothermic at -28,591 cal per g-atom (914°K).' These values are of the same order of magnitude as the heat of formation of many intermetallic compounds and as such clearly indicate that very strong bonding must exist between the solute and tin atoms in the liquid solutions. Rhodium might be expected to display similar solution characteristics in tin in view of its close electronic resemblance to palladium and platinum. Since no thermodynamic data are available for Rh-Sn alloys, rhodium was chosen as an appropriate solute for further investigation of transition-metal systems with highly exothermic heats of solution at infinite dilution. EXPERIMENTAL The heat of solution of rhodium in dilute Rh-Sn liquid solutions was measured as a functlon of rhodium concentration at 700°, 725", 750°, and 775°K. The liquid-metal solution calorimeter used in this work has been fully described elsewhere. At the start of each series of measurements, the solvent bath consisted of about 0.5 g-atoms of 99.9+ pct pure tin. To this was made a number of small rhodium additions, about 0.0005 g-atoms each, and the heat of solution was measured for each. Rhodium of 99.9+ pct purity in powder form was used in order to promote rapid dissolution in the liquid tin. The powder specimens were contained in tin foil stated to be purified (lead-free). This foil was found to have no measurable heat of solution in pure tin so the effect of any impurities could be neglected. The energy equivalent of the calorimeter was experi- mentally determined by dropping tungsten and/or tin specimens at intervals during each series of rhodium drops. The tungsten and tin used were 99.95 and 99.999+ pct pure, respectively. The only heat effect due to a tungsten drop, or a tin drop at low rhodium concentrations in the bath, is the sensible heat of the specimen. The heat content of these materials is well-established and is presented in the compilation of Hultgren et al. 4 As the rhodium concentration in the tin bath increases a small heat effect arises from the reaction: Sn (liquid, T) — & (soln, T) where T is the temperature of the tin bath. Where necessary, this heat of solution of tin was determined by Gibbs-Duhem integration, and corrections were made to the heat effect of the tin calibration specimens and the tin foil containing the rhodium specimens. RESULTS AND DISCUSSION The calculated values of the heat of solution of rhodium in dilute Rh-Sn alloys as a function of composition are shown graphically in Fig. 1. The values have been corrected for the sensible heat of the specimens, initially at 273"K, and apply to the reaction:

Jan 1, 1969

By Robert B. Coleman

The recent surge in demand for uranium in the US, accompanied by a significant increase in price, has stimulated the search for and development of lower grade ore bodies. At the mill, this translates into much larger throughputs and-compounded by many recently enacted environmental considerations-has made the cost of milling a critical factor in today's uranium production economics. The three conventional milling methods employed in the extraction of uranium ores are reviewed in the following sections.

Jan 10, 1978