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By D. V. Edmonds, C. J. Beevers

Tensile tests were carried out on a! titanium containing 850, 1250, and 2700 ppm 0, and up to -500 ppm H. The tests were performed at -196", -78", 20°, 150°, and 300°C at a strain rate of -1.0 x 10??3 sec-1. Increasing oxygen content, increasing grain size, and decreasing test temperature resulted in enhanced embrittlement of the a titanium by the hydrogen additions. Metallographic observations showed that this can be correlated with the influence of these parameters on the introduction of cracks into the a! titanium by fracture of titanium hydride precipitates. CRAIGHEAD et al.1 reported that the hydrogen content normally found in commercial-purity a! titanium (60 to 100 ppm) was sufficient to cause a substantial lowering of the impact strength, and they attributed this embrittling effect of hydrogen to the precipitation of titanium hydride. Lenning et al.&apos; found that in commercial-purity a titanium there is an almost complete loss of impact strength at about 200 pprn H, which is approximately half the value needed to eliminate the impact strength of high-purity a titanium. They also showed that the presence of 3000 ppm hydrogen reduces the room-temperature tensile ductility of commercial-purity material to a value of the order of 10 pct; the corresponding hydrogen concentration for high-purity titanium is over 9000 ppm. It thus appears that the detrimental effect of hydrogen on the mechanical properties of commercial-purity titanium becomes evident at much lower hydrogen contents than for high-purity titanium. The main difference between the two types of a titanium might be expected to be the higher level of interstitial impurity in the commercial-purity grade. Jaffee et a1.3 studied the influence of temperature and strain rate on the hydrogen embrittlement of high-purity and commercial-purity ! titanium. In general, the behavior was the same for both materials; embrittlement was enhanced by decreasing temperature and increasing strain rate. Recent results from tests on commercial-purity a titanium containing 850 ppm O and varying amounts of hydrogen up to -500 ppm showed that the degree of embrittlement by hydrogen is intimately related to the fracture characteristics of titanium hydride precipitates.4 The present paper considers the interrelationship between the mechanical properties and micro-structural features of commercial-purity a! titanium containing 850, 1250, and 2700 ppm 0 and varying amounts of hydrogen up to -500 ppm. 1. EXPERIMENTAL PROCEDURE Three types of commercial-purity titanium supplied by IMI* were used in the investigation, and for the *Address: Witton, Birmingham 6, United Kingdom. purpose of this paper are designated Ti 115, Ti 130, and Ti 160. The principal impurity elements are given in Table I. The material was received in the form of 12.7 mm diam bars having a fully recrystallized structure. Tensile specimens with a round cross-section of 4.5 mm diam and a gage length of 15.2 mm were machined from the bars. In order to develop the same grain size (mean linear intercept of grain boundaries) in each of the three types the specimens were annealed under a dynamic vacuum of <10?5 mm Hg, Table 11. Specimen hydriding was carried out in a modified Sieverts apparatus;&apos; hydrogen was taken into solution at 450°C and after holding the specimens at this temperature for 24 hr they were furnace-cooled to room temperature at an average rate of -100 C deg per hr. By this method nominal hydrogen contents of 0, 50, 100, 250, and 500 ppm were introduced into specimens of Ti 115, Ti 130, and Ti 160 (100 ppm (wt) -0.5 at. pct). The actual hydrogen contents were calculated from the weight differences obtained by weighing the specimens before and after the hydriding treatment. Tensile tests were carried out at temperatures of -196", -78", 20°, 150°, and 300°C on a 10,000 kg In-stron machine at a nominal strain rate of -1.0 x 10-3 sec-1. Fractured specimens were sectioned in planes parallel to the tensile axis, mechanically polished to 0.25 µm grade of diamond paste, and then attack polished using a solution containing by volume 99 parts H2O, 1 part HF, and 1 part HNO3. Although the latter treatment unavoidably opened out cracks and voids visible after mechanical polishing, it did reveal the grain structure, titanium hydride morphology, and deformation twinning structure.

Jan 1, 1970

By E. H. Rose

The question is often pondered whether the flotation process is still an art or has become a science. The fact is that flotation is a science in so many variables that only art can blend them. It is demonstrable that no less than one hundred variables are involved in any flotation operation, most of them immeasurable on a routine basis. The behavior of every one of them is always governed by orderly and unchanging law, as no man can doubt. There is nothing truly indefinite about that behavior; the only indefiniteness is in our knowledge of it, either in general or from hour to hour in the circuit. In dealing with a simultaneous equation in, say, one hundred variables, all not only affecting the outcome to some degree but many influencing each other as well, it is small wonder that the mineral-dressing profession presents a case history of debate and controversial opinion. The statement of the subject of this symposium—a symposium on flotation machines—seems to delimit and define the matters to be considered and at least the general nature of the conclusions sought. Nevertheless, in such a meeting it is not possible to meditate upon all the variables that do in one way or another affect performance of flotation machines. To attempt it would be much like trying to operate a hundred-ring circus. Perverse variables being what they are, one could expect the elephant in ring 36 to squirt a trunkful of water at the tightrope performer in ring 37 to ruin that artist&apos;s act, just as our learning to depress pyrite in the early 1920&apos;s ruined the act of the formerly faithful old Callows. Honest Disagreements Selective flotation dates from 1922 or 1923, when several plants established their regular flotation operations on a selective basis. Since then, two decades of efforr have gone into the development of better and better flotation machines. Many have come and gone. The competition has simmered down to perhaps a dozen machines, each one of which is staunchly defended by some operators as being the best for their particular jobs, and as scornfully dismissed by at least a few others elsewhere as being positively the poorest for theirs. These disagreements are honest disagreements, honestly arrived at after plenty of sweat. In many a flotation plant, one machine has been tried out against another under conditions as fair as they could possibly be made. Sometimes the results are on a par but more often one machine shows a consistent and unmistakable margin of superiority over the other. In equally honest and enlightened tests, machine A may win over machine B in one place, and machine B over machine A by as great a margin in another. This paper purposes to identify some of the more prominent reasons why this is so,

Jan 1, 1947

By Walter Miller

Petroleum refining, like other industries in the United States in 1940, focused much attention on its duties and opportunities in the field of national defense. In crdiiter-distinction to the situation during the World War, the industry is well constituted as to existing equipment, processes, and capacity, together with planned additions, to handle any demands that may be made upon it by the defense program needs. Evident throughout was the growing sense of ability to manipulate oil molecules for the production of materials not hitherto considered as being available commercially from petroleum. The development and application of catalytically induced reactions on a broad front is one of the distinguishing characteristics of refining progress during the year. In the hands of the refiner, catalysis has developed into a most important means to secure higher antiknock motor fuels and 100-octane fighting grade aviation gasoline in greatly increased quantity. One illustration of the importance being assigned to catalytic refining is the construction by the Houdry group of an experimental laboratory at a cost of $7&apos;307&apos;30&apos;3, to be staffed with over 100 research men7 solely for the purpose of studying catalytic reactions. In the aviation gasoline picture a modification of specifications by the Government widened the field from which acceptable fuel can be secured, and the continued expansion of the alkylation process in itself promises to go far in filling the demands expected from 50,000 fighting planes. It is conservatively estimated that eyen now the industry can turn out 1,300,000 gal. of 100-octane aviation gasoline daily. The upper limits of octane numbers for regular grades of motor gasoline reached in 1939 were not exceeded, but the average octane number approached the upper level more closely. A survey made of the 1940-model cars showed no rise in average octane requirement of the engines. The trend throughout the year was for greater reliance on the A.S.T.M. method for octane determination. The "1939 Research Method" is less widely used, although still considerably in evidence; the older L-3 method seems to have lost considerable ground and to be on the way out. Re-forming Capacities Increased Interest continued to grow apace in re-forming low-octane naphthas into high-octane gasolines. Some additions, although not great, were announced in thermal re-forming capacity. Interest in catalytic re-forming was greatly stimulated by the technical success of the operation of the converted hydrogenation unit at the Bay-way, N. J., rehery of the Standard Oil Company of New Jersey, mentioned in last year&apos;s review, and also by the knowledge that recoverable proportions of toluene are present in the hydroformed (catalytically

Jan 1, 1941

By Nicholas Kowall, K. L. Clark

Maximum furnace efficiency and close control of final steel composition demand that the steel melter be able to follow closely the variations in the carbon content of the bath. For many years, the fracture test has been used by melters for estimating carbon, because it requires only a very short time to pour a sample into a chill mold, cool it in water, break it with a sledge hammer, and observe the fracture. After long experience gained from the observation of such fractures, most melters are able to estimate the carbon content of steel with amazing accuracy, particularly in the lower carbon ranges. Notwithstanding the utility of the fracture test, there has been widespread interest in other methods for rapid carbon determination to supplement it and to ensure against possible errors in human judgment. Several methods, based upon measurement of magnetic properties as functions of carbon content, have been described in the literature1-6 and have been found to give reasonably reliable results in plant practice when scrap composition is known and controlled. A difficulty encountered in the use of analyzers of the magnetic type is that alloying elements do change the relationship between carbon content and magnetic properties and it becomes necessary to establish calibration curves for all the expected combinations of alloy residuals that are not oxidized in the bath. The work reported here is of an investigation of a method that is independent of alloying elements normally present in constructional steels, being based upon the relatively well-known fact that in plain carbon and low-alloy steels martensitic hardness is a function of carbon content alone. Work oF Other Investigators In I938, Burns, Moore and Archer published & curve? that showed that the hardness of martensite is a function of carbon from 0.10 to 0.50 per cent and is independent of grain size or alloy content, at least within the rallge found in construc-tional S.A.E. compositions. Some of the deeper hardening types investigated, however, contained carbon to a maximum of only o.2o per cent. Using this principle, Kern8 developed a method of rapid carbon determination for S.A.E 43xx steels, His procedure consisted of chill-casting a test bar that was large enough to give a a that could be prepared for Brinell indentations. The test piece was quenched immediately after solidi fication was complete and hardness readings were taken, so that the carbon content could he read from an experimentally determined curve giving the relationship between as-quenched hardness and carbon. Experimental Work Although Kern&apos;s work had been done with a relatively deep-hardening steel, it

Jan 1, 1944

By E. H. Rose

The question is often pondered whether the flotation process is still an art or has become a science. The fact is that flotation is a science in so many variables that only art can blend them. It is demonstrable that no less than one hundred variables are involved in any flotation operation, most of them immeasurable on a routine basis. The behavior of every one of them is always governed by orderly and unchanging law, as no man can doubt. There is nothing truly indefinite about that behavior; the only indefiniteness is in our knowledge of it, either in general or from hour to hour in the circuit. In dealing with a simultaneous equation in, say, one hundred variables, all not only affecting the outcome to some degree but many influencing each other as well, it is small wonder that the mineral-dressing profession presents a case history of debate and controversial opinion. The statement of the subject of this symposium—a symposium on flotation machines—seems to delimit and define the matters to be considered and at least the general nature of the conclusions sought. Nevertheless, in such a meeting it is not possible to meditate upon all the variables that do in one way or another affect performance of flotation machines. To attempt it would be much like trying to operate a hundred-ring circus. Perverse variables being what they are, one could expect the elephant in ring 36 to squirt a trunkful of water at the tightrope performer in ring 37 to ruin that artist&apos;s act, just as our learning to depress pyrite in the early 1920&apos;s ruined the act of the formerly faithful old Callows. Honest Disagreements Selective flotation dates from 1922 or 1923, when several plants established their regular flotation operations on a selective basis. Since then, two decades of efforr have gone into the development of better and better flotation machines. Many have come and gone. The competition has simmered down to perhaps a dozen machines, each one of which is staunchly defended by some operators as being the best for their particular jobs, and as scornfully dismissed by at least a few others elsewhere as being positively the poorest for theirs. These disagreements are honest disagreements, honestly arrived at after plenty of sweat. In many a flotation plant, one machine has been tried out against another under conditions as fair as they could possibly be made. Sometimes the results are on a par but more often one machine shows a consistent and unmistakable margin of superiority over the other. In equally honest and enlightened tests, machine A may win over machine B in one place, and machine B over machine A by as great a margin in another. This paper purposes to identify some of the more prominent reasons why this is so,

Jan 1, 1947

By Walter Miller

Petroleum refining, like other industries in the United States in 1940, focused much attention on its duties and opportunities in the field of national defense. In crdiiter-distinction to the situation during the World War, the industry is well constituted as to existing equipment, processes, and capacity, together with planned additions, to handle any demands that may be made upon it by the defense program needs. Evident throughout was the growing sense of ability to manipulate oil molecules for the production of materials not hitherto considered as being available commercially from petroleum. The development and application of catalytically induced reactions on a broad front is one of the distinguishing characteristics of refining progress during the year. In the hands of the refiner, catalysis has developed into a most important means to secure higher antiknock motor fuels and 100-octane fighting grade aviation gasoline in greatly increased quantity. One illustration of the importance being assigned to catalytic refining is the construction by the Houdry group of an experimental laboratory at a cost of $7&apos;307&apos;30&apos;3, to be staffed with over 100 research men7 solely for the purpose of studying catalytic reactions. In the aviation gasoline picture a modification of specifications by the Government widened the field from which acceptable fuel can be secured, and the continued expansion of the alkylation process in itself promises to go far in filling the demands expected from 50,000 fighting planes. It is conservatively estimated that eyen now the industry can turn out 1,300,000 gal. of 100-octane aviation gasoline daily. The upper limits of octane numbers for regular grades of motor gasoline reached in 1939 were not exceeded, but the average octane number approached the upper level more closely. A survey made of the 1940-model cars showed no rise in average octane requirement of the engines. The trend throughout the year was for greater reliance on the A.S.T.M. method for octane determination. The "1939 Research Method" is less widely used, although still considerably in evidence; the older L-3 method seems to have lost considerable ground and to be on the way out. Re-forming Capacities Increased Interest continued to grow apace in re-forming low-octane naphthas into high-octane gasolines. Some additions, although not great, were announced in thermal re-forming capacity. Interest in catalytic re-forming was greatly stimulated by the technical success of the operation of the converted hydrogenation unit at the Bay-way, N. J., rehery of the Standard Oil Company of New Jersey, mentioned in last year&apos;s review, and also by the knowledge that recoverable proportions of toluene are present in the hydroformed (catalytically

Jan 1, 1941

By G. D. Van Arsdale

THE paper of Mr. Posnjak presents a laboratory confirmation of the well known facts that air ox-idation of pure solutions of ferrous sulfate is slow and difficult and that, like many other similar reactions, the speed, may be greatly accelerated by the presence of other substances, often in very small amounts, the effect of the presence of copper being determined ex-perimentally in this case. However, it should not be. overlooked that copper is always present in heap leach-ing solutions in amounts equal to or greater than those in the experiments described; therefore the paper may be considered as an explanation of present results rather than a possible improve-ment to be added to present practice. It is not practicable and it does not pay to precipitate copper by ce-mentation below a point about 5 lb. per 1000 gal., equivalent to about 0.0005 mol. Cu. per liter, compar-ing with the approxi-mately 0.0009 mol. per liter of curve 2 in the diagrams given of course, also, in the heaps local concentrations are usually very much higher than this, which is also true of the effluent li-quors, so that I feel that it is safe to say that copper is already present in amount sufficient to realize, as large an accelerating effect as is practicable. Too much im-provement or refinement cannot be expected in a method of this kind, due to commercial limitations. It should be remembered that chemically and physically there is no sharp dividing line between leaching in place, heap leaching, and the usual tank leaching practice, practi-cally the same reagents being used in all three. From the viewpoint of extractions, etc., it is not common sense to apply leaching in place to an orebody carrying enough copper to pay for mining; and the same is true of heap leaching, for an ore carrying enough to pay for the crushing, handling, etc., of ordinary leaching. That is to say, leaching in place should properly be consid-ered only for an ore too low-grade to pay for mining, and heap leaching for the next higher grade, still how-ever too low-grade to pay for crushing and other re-finements. There is no advantage in leaching without mining or in heap leaching except lower cost of in-stallation and handling; on the other hand there are very distinct disadvantages which are inherent and which should prohibit their use except where necessity requires. The object of metallurgy is to make money out of the handling of ore, and it is purely a question of money as to how far we can go in "improving" or

Jan 7, 1927

By H. R. Stahl

THE disseminated lead district of Southeast Missouri lies 70 miles south of St. Louis. The only metal of economic importance in the ore is lead, but minor amounts occur of iron, zinc, copper, cobalt, nickel, silver and cadmium. These minor metals, as might be expected, tend to concentrate in both the flotation and table middlings. In the past, some zinc has been recovered by differential flotation. The silver and cadmium tend to associate with the zinc, and some recovery is made of these two metals at the smelter. The lead occurs as galena, or lead sulphide. The minor metals are also present as sulphides. The presence of oxidized lead is suspected, but has not been definitely proved. The gangue is chiefly dolomitic limestone, with small amounts of sandstone and shaly glauconitic and chloritic minerals. The ore contains about 3.25 per cent lead, occurring as galena disseminated through the gangue. Some of the galena is very finely disseminated, and the mineral in the gravity tailings, or chat, is seldom or never in the free state. The method of treatment of the ore has been evolved over a period of 75 years; hence probably is not far from correct. The milling processes have tended toward simplification during the past 15 years, but recoveries have never been sacrificed for the sake of simplicity. In many cases, simplification of flowsheets has led to better recoveries and operating economies. A simplified flowsheet is shown in Fig. I. The St. Joseph Lead Co. operates four mills in the Flat River district, with a normal total capacity of about 21,000 tons per day, divided as follows: Federal mill, 11,000 tons; Leadwood mill, 4500 tons; Desloge mill, 3400 tons and Bonne Terre mill 2400 tons. The methods of concentration used at these plants are similar in principle; they differ mainly in details and in the type and size of the equipment used. The process of concentration may be divided into five main steps; i.e., dry crushing, wet grinding, classification with its attendant desliming, tabling and flotation. A brief description of these processes will be given, noting important differences in the various plants, and also noting the more important changes or developments of the past few years. DRY CRUSHING The run-of-mine ore is hoisted in skips, the capacity of these skips ranging from 2 ¾ tons to 8 ¼ tons. At the Desloge plant, the ore is hoisted in 2-ton mine cars on self-dumping cages. All ore is hoisted at shafts adjacent to the various crushing plants, no ore being transported on the surface. Primary breaking at all the mills is accomplished with 9E Telsmith breakers. Preliminary screening is provided ahead of most of these crushers, either by station-

Jan 1, 1943

By Albert E. Reed

THE development of the modern high-speed vibrating screen, together with the increasing availability of long-lasting stainless-steel screen cloth for relatively fine-mesh separations, means that more screen circuits will be used in the future. It seems pertinent therefore to examine a few characteristics of screen-circuit products, and especially the points of difference as compared with products of classifier circuits. The most noticeable change that takes place when substituting screening for classification in a grinding circuit is a substantial drop in the circulating load, owing to the greater ease with which the "fines" leave the circuit. Where circulating loads of 500 to 600 per cent are considered fairly normal in classifier grinding circuits, the grinding circuit equipped with screens for equivalent work will have a circulating load of only 20 to 75 per cent. As a result, the products of screen circuits will show a minimum of overgrinding or sliming as compared with a classifier circuit. The desirability of this characteristic will naturally vary according to the metallurgical requirement in each case. Because screen separations make a sharper division according to particle size, the products of screen circuits can be expected to show greater crowding of particles near the point of separation. These changes in product characteristics are so important that other factors, both in the grinding and concentration processes must be adjusted if the operator is to take full advantage of the increased tonnages and higher efficiencies available to him through the use of the screen circuit. One factor that too often is overlooked when changing to screen circuits is the importance of adjusting the ball-mill or rod-mill charge, to compensate for: (I) increased tonnage of new feed, (2) decreased circulating load, or (3) more granular character of feed. These same factors should also be taken into consideration for their effect on the various types of concentration or flotation equipment that may follow the screen circuit. Over a period of years, this equipment has generally been designed and adjusted to the product of the classifier, therefore it seems obvious that some research on the adjustment and adaptation of concentrating and flotation equipment to screen-circuit products will be most profitable to the operators. To illustrate the points mentioned above, the results from three recent installations follow, with data on the comparative characteristics of screen and classifier circuits. A range of separation from 10 to 48 mesh has been chosen, using two general types of screening equipment and two types of classifiers. The first of the installations of which the results are to be examined is that of an iron-ore installation where eastern magnetite was being concentrated prior to sintering. Fig. I shows the original grinding circuit, using classification, while Fig. 2 shows the same circuit equipped with a

Jan 1, 1945

By K. L. Clark, Nicholas Kowall

Maximum furnace efficiency and close control of final steel composition demand that the steel melter be able to follow closely the variations in the carbon content of the bath. For many years, the fracture test has been used by melters for estimating carbon, because it requires only a very short time to pour a sample into a chill mold, cool it in water, break it with a sledge hammer, and observe the fracture. After long experience gained from the observation of such fractures, most melters are able to estimate the carbon content of steel with amazing accuracy, particularly in the lower carbon ranges. Notwithstanding the utility of the fracture test, there has been widespread interest in other methods for rapid carbon determination to supplement it and to ensure against possible errors in human judgment. Several methods, based upon measurement of magnetic properties as functions of carbon content, have been described in the literature1-6 and have been found to give reasonably reliable results in plant practice when scrap composition is known and controlled. A difficulty encountered in the use of analyzers of the magnetic type is that alloying elements do change the relationship between carbon content and magnetic properties and it becomes necessary to establish calibration curves for all the expected combinations of alloy residuals that are not oxidized in the bath. The work reported here is of an investigation of a method that is independent of alloying elements normally present in constructional steels, being based upon the relatively well-known fact that in plain carbon and low-alloy steels martensitic hardness is a function of carbon content alone. Work oF Other Investigators In I938, Burns, Moore and Archer published & curve? that showed that the hardness of martensite is a function of carbon from 0.10 to 0.50 per cent and is independent of grain size or alloy content, at least within the rallge found in construc-tional S.A.E. compositions. Some of the deeper hardening types investigated, however, contained carbon to a maximum of only o.2o per cent. Using this principle, Kern8 developed a method of rapid carbon determination for S.A.E 43xx steels, His procedure consisted of chill-casting a test bar that was large enough to give a a that could be prepared for Brinell indentations. The test piece was quenched immediately after solidi fication was complete and hardness readings were taken, so that the carbon content could he read from an experimentally determined curve giving the relationship between as-quenched hardness and carbon. Experimental Work Although Kern&apos;s work had been done with a relatively deep-hardening steel, it

Jan 1, 1944

By V. S. Tuman

In the first part of this paper, an estimate is made of the magnitude and extent of the thermal stresses which result from mud circulation. Our study is made for the period of relaxation, i.e., when the drilling operations are terminated and mud circulation is discontinued. In the second part, we have shown how the thermal stress can affect the wave propagation. An example is worked out for a Carbondale sandstone (Illinois basin). It is concluded that, in extreme cases when differential temperature is about 100°F, the travel time will be affected by about 2 microsec/ft. For more refined permeability studies, such corrections would be desirable. MAGNITUDE AND EXTENT OF THERMAL STRESSES RESULTING FROM MUD CIRCULATION When geological beds are penetrated by boreholes, it is observed that the formation temperatures increase with depth; however, the temperature profile varies considerably from place to place. During drilling operations, mud pumped from a pit at atmospheric temperature absorbs heat from the lower beds. As a result, the drilling fluid returning to the surface is at a higher temperature than the surrounding beds. The temperature gradient in a well depends on the rate of mud circulation and other factors; normally, this temperature gradient is smaller than the natural gradient in the formations. (See Fig. 1.) The temperature difference between the mud column and the surrounding beds gives rise to therma1 stresses (which are also important in the phenomenon of fracturing), and it is expected that they will affect the transit time of the sonic front in velocity logging.1 It is evident chat beds near the surface will undergo various cycles and will have a complicated dynamical and thermal-stress history. A limestone bed which is just penetrated will act as a source of heat, warming up the cold mud pumped down a few minutes earlier from the surface pit. The same limestone bed a week later will act as a sink, absorbing heat from the drilling mud which has already warmed up sufficiently to be at a higher temperature than the bed in question. No doubt a large section of the hole will undergo a heat treatment, which will make the calculation of the exact magnitude of the thermal stresses very difficult. In the solution of wellbore thermal equation, it is assumed that the rock around the wellbore is elastic and isotropic, and that the system is radially symmetrical. A complete dynamical solution of the thermal stresses set up at different horizons during the drilling operations would require a comprehensive history of the mud circulation, the surface temperature of the pit and the number of hours in which mud was not circulated. CONDUCTION OF HEAT AND THERMAL EQUATION OF STATE

By W. O. Philbrook, H. W. Hosking, N. B. Melcher

A simple and inexpensive mercury-tracer method has been develohed to study rates and Patterns of gas flow in blast furnaces. A Pulse of mercury is injected into the hot blast, and its arrival at the sampling Point is recorded by an electronic circuit that measures resonant absorbtion of ultraviolet light by mercury vapor in the gas aspirated .through the detecting. cell. A rapidly developing interest in blast-furnace technology in recent years has created a strong demand for precise knowledge of the rates and patterns of gas movement through the stock column. Classical fluid-flow theory cannot supply the desired information because the complexity of the blast-furnace situation precludes the accurate determination of many of the parameters required for solution of the equations. In fact some of the terms employed in fluid-flow treatments become almost meaningless under blast-furnace conditions. The void fraction of the stock column, for example, varies widely from place to place and is affected by the segregation of charge materials, attrition of lumps during descent, and channeling. Gas density varies with changes in local pressure, temperature, and composition, while viscosity varies with temperature and composition. Even if mean values for these functions were acceptable, they would be either impossible or extremely difficult to determine with a high degree of accuracy since the value of the mean for all gas properties would depend upon the flow distribution itself. Attempts to study gas movement by the pitot-tube determination of kinetic pressures have met with little acceptance. Reproducibility of results is extremely difficult to achieve in a situation where alignment of the tube orifice with respect to the flow direction in tortuous channels cannot be guaranteed. Because of these difficulties it would appear that progress can be achieved only with a direct method of measuring gas velocities and determining the shape of flow paths through the stock. The establishment of such a method is described in this paper. SELECTION OF METHOD Direct measurement suggests the use of a tracer by means of which the progress of a "parcel" of gas can be followed through the furnace. Several requirements must be met before any selected material can be considered a suitable tracer. First of all, it must be a substance not normally present in blastfurnace gas or dust; otherwise its presence in a gas sample will have little significance. It should be volatile at temperatures normally existing within the furnace, to ensure that it will travel with the gas, as a gas. It should possess special properties enabling its presence in the gas to be detected readily, and it should not undergo exchange reactions with any material normally present within the furnace, including refractories and coke as well as all components of the metal and slag. Radioactive materials naturally are considered because their radioactivity renders them susceptible to detection. However, of the many radioactive materials available, almost all are eliminated from final consideration by their unsuitability in terms of other properties. Radioactive silicon, carbon, calcium, phosphorus, and many others have been considered and discarded, either because they are not volatile over the whole range of significant temperatures, or because they could be expected to undergo exchange reactions with burden or refractory materials. Others which might be suitable in terms of these properties are eliminated because of a low activity, short half life, or the necessity for fragile counting apparatus. Of the many elements available in radioactive form, perhaps radon is the only one suitable for blast-furnace gas-flow studies. This has been used in several investigations1-4 with considerable success. The use of radiotracers has certain inherent disadvantages. One is the cost. An appreciable sum must be allowed for materials each time a test is made. Also, special methods of handling must be employed, and very often the progress of an investigation must be governed by the availability of isotopes and the delivery arrangements that can be made for them. An advantage is immediately gained if the tracer material can be a substance which can

Jan 1, 1960

By R. J. Mellen

IN a chloridizing roasting and cyanidation plant treating a manganese-silver ore, certain experiments pointed out the way to an improvement in roasting conditions by a change in the degree of crushing. The following short article is simply a description of the various changes that were necessary throughout the plant and of the results obtained. There is nothing unusual in these changes but they are of some interest in that they constitute a good many of the alterations usually resorted to in increasing production. In the beginning, the changes were brought about by an experiment that was not successful, but which clearly pointed to means of improving the operation, and is an example of the fact that often experimental work may result in failure and still be of value in arriving at correct fundamentals. This experiment also shows how far a metallurgist can get out of line in his deductions, particularly in a field with which he is not thoroughly familiar. The ore at the plant of Compania Minera Kildun y Anexas is crushed through a 13-in. gyratory, a 3-ft. standard Symons cone crusher and a set of 16 by 42in. rolls, the latter in closed circuit with two Tyler 400-mesh screens. The crushed ore is then conveyed to two fine-ore bins. These provide storage and feed for two 6 by 90-ft. kiln roasters, which discharge directly to coolers. The coolers in turn discharge to a 6 by 12-ft. ball mill, where the ore is ground for cyanidation. Laboratory and pilot-plant tests previous to the mill construction had indicated that minus ¼ -in. crushing was satisfactory for roasting, although results did not vary greatly with some coarser or considerably finer crushing. The plant was designed for a capacity of 300 tons per day on this basis. After a few months operation, the initial operating problems were overcome and the anticipated milling rate was reached but the results being obtained were not really good. The plant seemingly did not have much excess capacity in any department but the roasting operation was the most critically limiting factor both as to tonnage and the results obtained. If this could be improved there seemed some possibility of improving the total tonnage rate to some extent. Segregation of the calcine into various screen sizes showed that the coarser sizes ,were not giving the expected recoveries. In all of the laboratory and pilot-plant testing, any limiting conditions as to the percentage of salt used, temperatures, feed rates, etc., had affected the fine material more than it had the coarse, and even in making laboratory tests at this time the mill conditions could not be exactly duplicated. Further laboratory testing indicated that a segregation of the crushed ore into a coarse and fine product for roasting might result in some improvement in roast-

Jan 1, 1945

By Emma Smith, R. W. Guard

INVESTIGATION of the nickel-rich end of the Ni-Zr system has been prompted by an interest in the effect of small amounts of zirconium in high temperature alloys. Hansenl presents a hypothetical diagram based on the work of Allibone and Sykes,2 who investigated the system up to 44 atomic pct (55 wt pct) Zr by metallographic means. Since the alloys they used were melted in Alundum crucibles they were probably contaminated with appreciable amounts of aluminum. They found two compounds which they called Ni3Zr and Ni4Zr. Hayes, Roberson, and Paasche3 identified a compound NiZr (50 atomic pct Zr) with a melting point of 1470°C. Such a high melting compound is not compatible with the observation of Allibone and Sykes2 hat a eutectic is formed near 50 atomic pct. The alloys containing up to 60 atomic pct Zr were melted in an inert atmosphere in a noncon-sumable electrode arc furnace. Analysis of most of the alloys indicated negligible loss of zirconium. The alloys were examined in the as-cast condition and also after annealing for 6 hr at 1175°C (or 1000°C for the alloys between 25 atomic pct and 45 atomic pct). Metallographic specimens were etched using mixtures of HF-HNO3-H2O or acetic acid- HN0,-H,O. The specimens for the solidus determinations were wrapped in molybdenum foil and sealed in evacuated quartz tubes. Specimens to be heated above 1300°C were enclosed in zirconia tubes inside the quartz to prevent reaction with molybdenum. The solidus determinations were carried out by heating the specimens at various temperatures for a few minutes and then examining the interior structure metallographically to determine at what temperature melting began. The 150 mesh powders for X-ray analysis were annealed in an evacuated quartz tube for 2 hr at 540 °C to remove cold work. Alloys with 22.5 atomic pct Zr and 44.4 atomic pct Zr required annealing at 700 °C for complete recovery. The grains of both of these alloys were soft and rather ductile. Both Debye-Scherrer film patterns and spectrometer traces were made for each alloy using filtered copper radiation. Results and Discussion The presence of a substantial amount of second phase in an alloy with 1.1 atomic pct Zr indicated that the solid solubility of zirconium in nickel is somewhat less than 1 atomic pct. The a0 value for the face-centered-cubic matrix in the same alloy was equal to that of pure nickel, so that the solubility must be very small. This observation is as expected from the large atom size difference. Annealed specimens of alloys with 15.0, 16.7, 22.5, 28.6, 44.4, and 59.4 atomic pct Zr showed. micro-structures that were essentially single phase. When

Jan 1, 1958

By A. S. Nowick, C. Y. Li

It is deMonstrated that quenching from an elevated temperataupe accelerates the grain boundary relaxation in two solid solutions (aAg-Zn and a Cu-Al). This result is consistent with the proposal that, in solid solutions, grain boundary relaxation occurs by a mechanism of&apos; self diffusion. Nevertheless, an alternative possibilitg, that quenching introduces vacancies into the boundary itself, must also be considered. THE phcnomenon of grain boundary relaxation has been well known for many years,1,2 yet the mechanism of this process is very poorly understood. One of the most interesting suggestions which relates to the mechanism of grain boundary relaxation was that of Ke,3 who claimed that the activation energy for grain boundary relaxation and for lattice self diffusion were essentially the same. The implication is therefore that the elementary step in the two processes is the same. This suggestion is particularly startling in view of the fact that activation energy for self diffusion along a grain boundary is very significantly lower than that for volume self-diffusion. Later evidence5-7 showed that there really are two grain boundary peaks, one which appears in high-purity metals, and the other (which develops at a higher temperature than the first) which appears in solid solutions beginning at solute concentrations in the range of 0.1 pct. Data for silver6 show that Kg&apos;s hypothesis is surely incorrect for the grain boundary peak in the high-purity metal, since it has an activation energy of only 22 kcal per mole, but that the hypothesis may still be correct for the grain boundary peak in various silver solid solutions, for which activation energies in the range 40 to 50 kcal per mole are observed. If the elementary step in the grain boundary relaxation process were the same as that for self-diffusion, it would be expected that the relaxation process could be hastened by quenching, 2.c. by introducing a non-equilibrium excess of lattice vacancies. Such a quenching effect has already been demonstrated in the case of another anelastic relaxation process, viz., the Zener relaxation effect. The Zener effect, which occurs in essentially all solid solutions, may be attributed to the reorientation of pairs of solute atoms in the presence of an applied shear stress,&apos; and therefore must take place by means of a volume diffusion mechanism. The hastening of this process through quenching9 has been one way of demonstrating that atom movements in the lattice take place through a defect mechanism, presumably single vacancies. In order to see if the grain boundary relaxation is affected by quenching, it is particularly convenient to compare the grain boundary relaxation with the Zener effect, by choosing a specimen for which both relaxation effects appear. Specifically, a fine-grained sample of a solid solution shows in the curve of internal friction vs temperature, first a peak due to the Zener effect, then a second rise (and eventually a peak at substantially higher temperatures) due to the grain boundary relaxation. The same phenomena are also observable in static anelastic measurements, such as creep at very low stress levels. Thus, for the same fine-grained solid solution, the creepstrain, when plotted against log time, falls on a sigmodial curve with a sharp inflection point, due to the Zener effect, which is followed by a second rise and inflection resulting from the grain boundary relaxation. To look for a quenching effect, static measurements are preferable to the dynamic internal friction measurements, due to the fact that quenching effects tend to anneal out too rapidly at the temperatures at which the internal friction is measured.9 RESULTS AND DISCUSSION Creep experiments in torsion were carried out in an apparatus similar to that described by Ke1, whereby a wire is held under constant torque and its angular displacement is observed as a function of time. The alloy Ag-30 at. pct Znwas selected because of the large Zener relaxation that it displays. The two samples used were a "coarse grained" wire with a mean grain size about twice the diameter of the wire (diam = 0.032 in.), and a "fine-grained" wire which had several grains across the diameter. In Fig. 1 a comparison is made of the creep curves at 160°C of these two samples after they had been cooled slowly from 400°C. Curve A, which represents the coarsegrained sample, shows a unique relaxation process due to the Zener relaxation, with a relaxation time, T , in the vicinity of 100 sec. Curve B, which represents the behavior of the fine-grained sample, on the other hand, shows first the same relaxation process as that in A, followed by a turning up of the curve which corresponds to the onset of a second overlap-

Jan 1, 1962

By Wieland D. R., Hurst R. E., A. R. Hendrickson

Analysis of acidizing techniques, in correlation with reservoir data and a backlog of past treatments, has resulted in the development of a valuable engineering guide for planning acidizing treatments. Such treatments fall into three categories: (I) acid injection into the pores of the matrix; (2) acid injection into natural formation fractures at less than parting pressure; and (3) combination acidizing-fracturing treatments in which acid solutions (without propping agents) are injected at treating pressures sufficient to open and extend fractures through which the acid flows. Because the spending tirnze of acid during a specific well treatment does not change appreciably, maximunl penetration is attained when the first increment of injected acid is completely spent. Additional acid injection cannot be expected to further extend the benefits of the treatment. Depth of penetration will depend upon the reaction rate of the acid under treatment conditions, the injection rate of the acid into the matrix or fractures and the area-volume relationship existing in the flow channels. Based on Darcy&apos;s flow formula, extremely low injection rates must be used in order to keep bottom-hole injection pressures below formation fracturing pressure. As a result, only limited penetration of unspent acid will occur. Treatment records indicate that, in most acidizing treatments, formation parting pressures are exceeded, greatly extending acid penetration. Under these conditions, stimulation benefits are limited to the fracture area produced during the spending time of the first increment of acid injected into the formation. This area may be calculated from laboratory and well data to estimate depth of penetration. This, in turn, may be correlated with productivity data to assist The art of gas and oil well acidizing has been characterized by many changes in treating materials and techniques since its inception. These developments have been designed to provide greater production increases. prolong production declines and shorten payout time. Such improvements have been based primarily on data derived from laboratory research and field experience. As more of the variables influencing these treatments have been recognized and evaluated, acidizing has become less of an art and more of a science. Recent studies of fracturing treatments,&apos; in light of individual well conditions and the results of thousands of fracturing treatments, made possible the formulation of an engineering guide that is now being used to select optimum treating techniques and to forecast probable results of such treatments. A similar analysis of the factors controlling acidizing treatments has been made and is the basis for this paper, The findings herein can be used as a guide in the selection of acidizing solutions and techniques, tailored to fit specific well conditions and to provide optimum stimulation per dollar cost. Acidizing treatments may be classified into three basic categories—(1) treatments in which the acid is injected uniformly into the pores and flow channels of the matrix, (2) treatments in which the acid enters natural fissures and fractures in the formation at less than fracturing pressures and (3) injection of acid into the formation at a pressure sufficient to open and extend fractures into the rock through which the acid penetrates (without the inclusion of a propping agent). TYPE 1 — MATRIX ACIDIZING This category consists of treatments in which acid solutions are injected into a homogeneous carbonate

By H. M. Otte

Certain choices for the shear elements of the inhomogeneous distortion in the phenomenological theory of martensite formation are examined for their agreement with crystallographic and X-ray data of iron alloys. The assumption that the shear elements must represent slip or twinning systems characteristic of bcc metals is found to covey all observations, even when a small uniform dilatation is taken into consideration. In bct martensite, (011) becomes a possible twinning or faulting plane, in addition to {112), and qualitatively similar X-ray line broadening is to be expected from both. The basic concept inherent in the current theoriesl-4 of the formation of martensite is that the interface between the parent (austenitic) and product (martensitic) phase is an invariant strain plane (i.e., one that is undistorted and unrotated). Experimental evidence that the interface is of such a nature is available in certain transformations2&apos;5&apos;6 but for the transformation in iron alloys direct observation has not proved enlightening. Internal strains resulting from the formation of the small martensite platelets within the parent austenite matrix7 make it difficult to produce the desired evidence. Indirect evidence, however, such as the continuity of scratches in passing from untrans-formed to a transformed region, strongly indicates that the habit plane in iron alloys is an invariant strain interface. The scatter in habit planes in a given specimen8 would suggest that internal stresses have a slight but definite influence. On the other hand, composition changes which affect the lattice parameter can alter the habit plane appreciably, and by an amount greater than the scatter.&apos; The success of the theories depends on the choice made for the "inhomogeneous distortion" or "complementary shear&apos;&apos; in the analysis and also on the choice for the parameter 6 representing a small uniform dilatation. In the approach developed by Wechsler, Lieberman, and Read&apos;," it is implicitly assumed that 6 is unity. In the case of iron alloys, all observations cannot be explained without varying either the inhomogeneous distortion or 6 . Bowles and Mackenzie3 considered only the effect of varying d. They found it difficult to reconcile the wide scatter of habit planes with the theory and were forced to the conclusion that it may also be necessary to consider variations or different choices of the inhomogeneous distortion. Wechsler and Read" considered a limited number of possible choices for the inhomogeneous distortion, but no variation in 6, though this could easily have been introduced if so desired. It is the purpose of the

Jan 1, 1961

By A. K. Jena, M. O. Bever

The thermodynamic behavior of dilute solutions of copper, silver, and gold in liquid tin is not explained by current solution theories.1-3 The relative partial gram-atomic enthalpies, or heats of solution, of silver, gold, and platinum in liquid lead at 623°K have been measured in the investigation reported here. Their interpretation requires a modification of the regular-solution theory although lead-rich solutions may be expected to be simpler than tin-rich solutions. The liquid metal solution calorimeter used has been described.4 At the start of a run the bath consisted of 621 g of reagent-grade lead. Several calibrating additions of lead were made during a run; a value of 3.48 kcal per g-atom5 was taken for H623°K - H273°K Two runs were made with each of the solutes silver, gold, and platinum. Annealed wire samples of 99.999+ pct purity were used. Four to six samples each weighing 0.5 to 1,0 g were added from 273°K to the bath at 623°K and the associated heat effects were measured. The samples dissolved in approximately 3 min. No serious experimental difficulties were encountered. The heat effects of the additions in a run plotted against the average atom fraction of solute before and after each addition314 were linear functions of the concentration in lead of silver, gold, and platinum, respectively. By subtracting the difference between the heat contents of a solute element at 623° and. 273°K5 from the measuredheat effects, the partial gram-atomic enthalpy relative to the solid solute was obtained. The relativ: partial gram-atomic enthalpy at infinite dilution and the concentration dependence of the partial gram-atomic enthalpies obtained from the plots of vs atomic fraction x are listed in Table I. The relative partial gram-atomic enthalpy at infinite dilution of silver in lead of 5.46 kcal per g-atom at 623°K compares with values at 723°K of 5.74&apos; and 5.765 kcal per g-atom. These data yield a temperature coefficient of 3.0 cal per g-atom-OK. The partial gram-atomic enthalpy at infinite dilution of gold in lead at 623°K is 0.89 kcal per g-atom compared with 0.85 kcal per g-atoms (obtained by extrapolation) and 0.95 kcal per g-atom.5 By combining these values for 623°K with those for several other temperatures5" the temperature coefficient of was found to be 3.2 cal per g-atom-OK. No thermodynamic data are

Jan 1, 1968

By D. K. Crampton, H. l. Burghoff, J. T. Stacy

THE effect of cold-working upon electrical conductivity of copper and of copper alloys appears not to be generally known in detail Although several papers on the subject have been presented, showing variable effects according to alloy composition, it is often assumed that the 2 to 3 per cent lowering of the conductivity of ordinary tough-pitch copper by severe cold-working is typical for copper alloys Because of this situation it was decided to carry out the present work upon several types of copper, copper-zinc alloys over the commercial range of brasses, other binary alloys, and numerous age-hardening alloys in the quenched, and quenched and aged conditions The large number of alloys investigated made it impossible to study every one in the detail it may have merited Inasmuch as several interesting points that could not be satisfactorily explained came to light, further work is contemplated by the authors It is usually considered that the normal effect of cold-work on ductile metals and unordered alloys is to decrease conductivity slightly In alloys that are in the ordered state, as annealed or otherwise heat-treated, cold-working tends to disorder the structure, resulting in very marked lowering of conductivity The random state of atomic arrangement produces lower conductivity than the ordered state for the same composition 1 PREVIOUS WORK previous work in the authors&apos; laboratory has shown the electrical conductivity of several copper alloys to be decreased by greater amounts than might have been expected, in view of the general knowledge on the subject, when cold-worked Guillet and Ballay2 investigated the influence of cold-work upon the resistivity of several metals and alloys, including copper and some copper alloys The increase of resistivity due to severe working was less than 4 per cent for all pure metals tested, while the increases for the alloys were generally higher In the copper-zinc alloys, they found that the increase of resistance due to drawing increased with zinc content, and reported a 21 7 per cent increase of resistance for an alloy containing 67 9 per cent Cu as severely worked Masima and Sachs3 studied the change in electrical resistance of three brass crystals when stretched in the tensile test, obtaining increases in resistance of the order of 3 per cent for 30 to 40 per cent reduction of area of the specimens The resistance decreased again when the cold-worked crystals were subsequently annealed Bardenheuer and Schmidt4 found that the conductivity of copper was decreased by 3 to 4 per cent when reduced 50 per cent by working The conductivity of 72-28

Jan 1, 1941

By John W. Bell

IN the introduction to an excellent pamphlet, John Gross1 makes the following statements: Although marked progress has been made along mechanical lines, the theory and conception of underlying principles have not advanced so rapidly. This lack of advance in theory may be attributed to the unfortunate situation resulting from the controversy as to whether the Rittinger or Kick law is applicable to crushing. Many pages of the technical literature are burdened with theoretical discussions in favor of one or the other of these laws, which have tended to cloud rather than to clear the atmosphere. Realizing the situation, the Milling Committee of the American Institute of Mining and Metallurgical Engineers, through its secretary, E. A. Hersam, studied the milling industry and, because of the apparently hopeless lack of agreement in the Kick versus Rittinger dispute (5, 13, 14, 16, 18, 19, 21, 22, 23, 24, 30. 34), concluded that a foundation for the theory of crushing was of primary importance. The numbers in the paragraph quoted refer to papers listed by Mr. Gross in his Bibliography on Crushing and Grinding.1 One is obliged to infer that these papers show "hopeless lack of agreement in the Kick versus Rittinger dispute." No. 22 is a paper by Arthur O. Gates2 and No. 23 is one by the writer.3 Employing the subject matter contained in papers Nos. 22 and 2323 the writer will show that their authors formulated identical conclusions, based solely on experimental evidence. Exactly the same defect in the Stadler hypothesis was described in each of the two papers, although entirely different experimental methods were employed in uncovering it. Both of the authors, independently, formulated the conclusion that Rittinger&apos;s was a. true hypothesis and Stadler&apos;s false. The evidence in a third paper4 will be employed to prove that Stadler&apos;s hypothesis, when examined experimentally, is worthless. STADLER&apos;S HYPOTHESIS WORTHLESS It is the writer&apos;s opinion that the evidence available in 1915 and the corroborating evidence in 1916 was amply sufficient to eliminate the need for any further consideration of Stadler&apos;s hypothesis. Certainly the evidence produced in 1918 dealt this hypothesis its coup de grace. It follows, therefore, that in the year 1918 there was only one credible hypothesis left-the Rittinger hypothesis. Gates&apos; Opinion What information is available in Mr. Gates&apos; paper?2 His conclusions are not consecutively summarized, none the less they are perfectly clear. On page 876, Gates says, and it is a very significant utterance: But my results show, among other things, that many more of Stadler&apos;s energy units are obtained per foot-pound-applied in coarse than in fine crushing. This suggests a doubt as to the correctness of his unit, since one would expect a foot-pound-applied to produce the same number of "energy units," whether the feed and resulting product were coarse or fine. When Rittinger&apos;s theory is applied, the number of mesh-tons (my unit of surface produced) is

Jan 1, 1942