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By Joseph E. Pogue

In 1920, 531 million barrels of crude petroleum were coi~sumed in the United States. As imposing as this figure is, the fact that the domestic consumption of crude petroleum has increased at an average rate of 10 per cent. a year for the past decade is more striking. Will this rate of increase in demand continue? If so, the year 1930 will call for 1260 million barrels of petroleum—a staggering volume. On the other hand, may we expect the demand for petroleum to grow as rapidly as it did when the automotive industry was having its most phenomenal expansion? If not, to what extent will the growth of oil requirements decrease? When and to what degree will the petroleum industry become affected by the economic law of diminishing returns? Obviously, this matter requires careful analysis, especially as both national and industrial planning must be predicated upon present estimates of the requirements of the future. The purpose of this paper, accordingly, is to project, as closely as present limitations of knowledge permit, the course of the demand for petroleum in the United States over the next ten years. At first, the problem of estimating the future of a demand as complex as that for petroleum might appear insoluble. Fortunately, hon~ever, therc are several scientific methods of approaching the problem, centering around a study of rates of industrial growth, which lend considerable hope that the requirements of the immediate future in this field may be approximated with sufficient closeness to have practical value as a basis of action. Growth oF Petroleum Demand The demand for crude petroleum is the resultant of the demands for the products made jointly from this substance—gasoline, kerosene, gas and fuel oil, and lubricating oils. The demands for these have grown at

Jan 1, 1923

By L. D. Anderson

WHEN, after years of troublous experiences in roasting sulfide ores with heavy dust and fume losses resulting from the equipment and methods first available, there appeared on the scene of metallurgy that revolutionary process known as sintering, it was felt that at last there had been found the ideal method for preparing sulfide ores for blastfurnace reduction. Not only were the sulfides roasted but also the fine oxidized ores were bound together with them in strong porous cellular masses which were in the best possible condition for reduction. With the experiences gained in the manipulation of the Huntington-Heberlein, Carmichael-Bradford, and Dwight & Lloyd processes there developed a refinement of detail which brought the whole plan of roasting by sintering to a high plane of perfection. But that metallurgy is never stationary is revealed by the fact that changes in milling practice, particularly the development of flotation, have introduced a new set of problems in sintering itself. Inasmuch as it is felt that these problems have not yet been solved in an entirely satisfactory manner this paper is written to record the present practice of the Salt Lake Valley smelters with the hope that there will be brought forth such discussios as may perhaps lead to still better practice. By far the greater proportion of the sulfides smelted today are flotation concentrates. Usually they are high grade, sometimes as high as 70 per cent. and more in lead. They are extremely fine, many mills grinding the ore so that from 60 to 80 per cent. will pass through screens of 200 mesh. The physical condition in which many of these concentrates reach the smelters is disconcerting to the metallurgists. Some are of about the consistency of putty. Others are of a sticky, slimy nature. Others again, dried to the limit, are veritable powders. Remembering that the down-draft sintering charge for the best results must be porous enough to let air be drawn through it reasonably well, must be thoroughly mixed, and must have some coarse material in it to segregate out and form a layer on the grates, it will be understood that the advent of this extremely fine material has made necessary still further elaboration in the equipment and processes of preparing sulfides for the blast furnaces,

Jan 1, 1929

By P. L. De Bruyn

The adsorption density of dodecylammonium ions at the quartz-solution interface has been Theadsorptiondensitydetermined as a function of collector concentration and pH. A ten thoushasbeenandfold range of amine salt concentration was covered at neutral pH. Experimental results show that over a thousandfold concentration range at neutral pH, the adsorption density (I) is proportional to the square root of collector concentration. Except at high concentrations, I increases with increases with increasing pH, but in general this effect is surprisingly small. . , . . A critical pH curve has been established for the flotation of quartz with dodecylammonium acetate. The conditions along the flotation curve are correlated with the adsorption measurements. THE behavior of collectors at the mineral-solution interfaces is usually explained in terms of an ionic adsorption process. Through the distribution of collector ions between the solid surface and the- co-existing solution phase the mineral is believed to acquire a water-repellent surface coating. Quantitative adsorption studies have been made on simple flotation systems1-4 only within the last few years. Such investigations were made possible by the adoption of the radiotracer method of analysis. As a consequence of these studies a new parameter has been added to aid the understanding of the flotation process. The research investigation to be discussed in this paper was undertaken to obtain a better understanding of the behavior of a cationic-type collector. This objective was approached through the determination of the distribution of dodecylammonium acetate between the quartz-solution interface and the solution as a function of the collector salt concentration and pH. To bring this investigation to focus on the more practical aspect of flotation research, an attempt was also made to correlate the adsorption results with actual flotation tests. Quartz: A —100 mesh ground crystalline quartz was infrasized; the products of the third and fourth cones were mixed together and reserved for experimental purposes. This stock material was cleaned by leaching in boiling concentrated HC1. After leaching the quartz was rinsed with distilled water until the filtrate showed no trace of chloride ian. It was then washed several times and dried. The qwrtz had a specific surface of 1400 cma per g as deterhined by the krypton gas adsorption method. Collector: The distribution of dodecylammonium acetate between the quartz surface and the solution phase was determined by the radiotracer method of analysis with carbon 14 as the tracer element. The radioactive amine salt with C" synthesized into the hydrocarbon chain5 was supplied by Armour and Co. The tracer element was located adjacent to the polar group. The radioactive salt as received had a specific activity of about 0.14 mc per g. When desired, dilution of this activity was effected by addition of non-radioactive dodecylammonium acetate also supplied by Armour and Co. ........ All other inorganic reagents used in this research were of reagent grade. Conductivity water was used for making up all solutions. Adsorption Tests: Two different experimental methods were used. In the first, to be designated as the agitation method, a weighed amount of quartz and a measured volume of amine salt solution were agitated in a 100-ml or 50-ml glass-stoppered pyrex graduated cylinder. The cylinder was filled with solution up to the stopper, since erratic results were obtained when an air space was left over the suspension. Time of agitation varied from 1 to 2 hr. Preliminary tests at different agitation times showed that the amount adsorbed remained constant for all agitation times exceeding 1/2 hr. After this conditioning period, the solids were separated from the solution by filtration through a Buechner fritted-disk funnel. The solution was re-circulated 10 times or more to allow the fused silica disk to come to equilibrium with it. Determinations of the amount of amine adsorbed on the frit itself indicated that this amount was less than 10 pct by weight of the amine acetate abstracted by 10 g of quartz. The funnel with quartz covered by a thin layer of solution was then centrifuged for approximately 5 min, at which time the moisture content of the solids was reduced to about 5 pct by weight. The wet quartz was blown into a tared beaker, re-weighed and allowed to dry at room temperature. A final weighing was then made to determine the moisture content. The second experimental method, similar to the procedure adopted by Gaudinand Bloecher,' will be referred to as the column method. Two liters of solution were passed through a bed of quartz contained in a Buechner funnel attached to a pyrex separatory funnel by means of a ball and socket joint. Preliminary tests showed that increasing the volume of solution above 2 liters does not give a measurable increase in adsorption. From 4 to 4 1/2 hr were required for 2 liters of solution to pass through the column. The moisture content of the quartz was again reduced to a minimum by centrifuging. A slightly modified column apparatus was used for experimenting with alkaline amine solutions. The same basic unit was used, but the underflow from the Buechner funnel was again fed into a Separafory

Jan 1, 1956

By G. P. Gladis, R. H. Atkinson

PALLADIUM has been used for jewelry for many years, particularly in conjunction with gold. This use increased in amount during the war, as palladium and gold were only moderately used for war purposes while demands for platinum and some of the other members of the platinum group were so great that their use in jewelry was prohibited. Palladium hardened with a small percentage of ruthenium has the necessary technical properties and appearance for good jewelry, and it is sufficiently rare to be desirable for luxury items-at least 100 times as rare as gold. Although both visual and spectrophotometric examination demonstrated that the color of palladium was almost the same as that of platinum, a few jewelers found the surface of palladium, even after some polishing, rather dark in areas that had been repeatedly heated during the soldering necessary to assemble certain types of handmade ornaments. This phenomenon is not to be confused with the thin, bluish oxide film that can be produced by heating in air over the range 400° to 800°C., as that film is easily reduced by dipping in warm 5 per cent formic acid or in warm methanol. It was suspected that the difficulty arose from heating in atmospheres that were alternately oxidizing and reducing, as Wise and Vines1 had found that this opened the grain boundaries of palladium and palladium-silver alloys in the same manner as in pure silver, as reported by Martin and Parker.2 This damage is caused by the reaction between oxygen in solid solution in the metal, acquired when heated under oxidizing conditions, and hydrogen diffusing in from subsequent heating under reducing conditions; the steam cannot diffuse out and therefore builds up sufficient pressure to disrupt the metal near the surface. Copper and various other metals can be damaged similarly, but platinum is nearly immune; therefore the problem was new to the platinum jeweler. Sulphur in the fuel gas also can cause trouble but did not appear to be dominant in the present instance. Metallographic examination of both pure palladium and ruthenium-palladium showed that the usual torch using oxygen and city gas as normally operated did in fact cause the surface and subsurface damage that had been observed, and also disclosed that a reducing flame caused more damage than an oxidizing flame and was very damaging even in the absence of any intentional swing in atmosphere from oxidizing to reducing (Fig. 7); besides the surface damage, there was serious loss of ductility. A full explanation of the mechanism of attack is not evident at the moment, but may be allied to the attack that occurs on heating catalytically active metals in nonequilibrium atmospheres.

Jan 1, 1946

By R. G. Hall

The method of crushing rock by throwing with violence against a resisting surface does not differ in principle from the method of dropping it from a height upon a specially arranged surface. The former is applied in various mills now in use, especially those for reduction of the softer rocks and minerals. The latter is the principle of the Hadsel mill. Probably not new, but Hadsel's method of approach is at least novel, and applicable to hard as well as softer rocks. An elevating wheel raises the rock and drops it from a height upon a hard metal plate or series of plates. The first commercial mill consisted of two units, one on each overhung end of a horizontal shaft, driven by a gear train from a 100-hp. motor. A description of this machine, then in operation at a mine at Georgetown, Calif., was printed in the Engineering and Mining Journal (April, 1932) and need not be repeated here. That machine took mine run ores of a size up to 12 in. and successfully produced a pulp of approximately minus 60 mesh, suitable for flotation. The mills were each 24 ft. in diameter and 3 ft. in width of face. The elevating buckets were formed of steel plates, extending inward from the periphery, inclined to the tangent at 75". This plate was 3 ft., the width of the wheel, and 2 ft. deep. One side of the wheel towards the carrying shaft was closed, the other was open except for the rim plate enclosing the ends of the buckets and extending inward about 5 ft. on the radius. About a 90" arc was immersed in a concrete tank, which acted as a classifier. The breaking plates, seven in number, were carried cantilever through the open side of the wheel. The lowest plate was placed just above the water level. The illustrations (Figs. 1 and 2) make plain the general arrangements. The plant set-up was somewhat crude but worked well enough to demonstrate the weak points of the mill. In this operation it was early apparent that, considering all the factors from delivery of the mine run ore to the final pulp for flotation or cyanida-tion, the Hadsel mill offered possibilities of great simplicity of plant and savings in power. Continuous operation developed mechanical weaknesses, some of which were readily discernible in details of design, some became more apparent as operations progressed.

Jan 1, 1935

By R. E. Zinkham, R. J. Goodwin

A mathematical study has been made of the amount of support a cement sheath could provide to casing cemented into the earth. Several assumptions were required to make the analysis, but only two of them are limiting: (I) the pipe must be completely surrounded with cement, and (2) any mud filter cake between the cement and formation has the same physical properties as either the cement or formation. The calculations showed that little support would be provided to the pipe before an unsupported cement sheath failed in tension; however, when the cement is confined between the pipe and wellbore and is loaded in compression, the pipe could receive a considerable amount of support. In fact, the theoretical results indicate the lower grades and larger sizes of pipe could have their working pressures doubled when reasonable compressive loads were applied to a surrounding cement sheath. These data are shown in six charts. Other down-hole conditions such as setting the cement under pressure, increased temperature and cement confinement all tend to increase the potential usefulness of the sheath. Because of size limitations, a laboratory program to verify the most important results of this mathematical study would be very difficult. However, small-scale field tests would be practicable. This paper shows that, if a solid cement sheath can be obtained in the field by either primary cementing or by repair after detection of flaws by surveys such as the new cement-bond logs, the use of this approach to reducing pipe costs merits further consideration. INTRODUCTION A modification in casing design practices is proposed which may either reduce the amount and grade of steel required to contain a specified internal pressure or permit the working pressure to be increased for a specified weight and grade of pipe. One of the more important considerations in casing design is its resistance to collapse; however, Bowers' and, more recently, O'Brien and Goins' have shown many casing programs are unnecessarily conservative in this respect, and they have indicated how savings can be made by designing for more realistic down-hole conditions. Earlier, Saye and Richardson howed that pipe costs could be reduced by considering the cement sheath as a part of the casing string when collapse resistance was being calculated. More recently, Rogers4 has raised the question as to whether a cement sheath might be considered in the design for burst resistance of the cemented casing. Calculations have been made for the increased burst resistance a cement sheath would provide for casing in a wellbore, and the results show that a sizable amount of support could be obtained in some instances. These data are presented in addition to a discussion of several other factors that are considered to affect the burst strength of pipe supported by cement. Two types of support are treated: Case I for tensile loading of the unconfined cement sheath, and Case for compressive loading of the confined cement sheath. ANALYTICAL TREATMENT AND RESULTS CASE I—TENSILE STRESSES IN AN UNCONFINED CEMENT SHEATH Conditions like this would most likely occur in a greatly enlarged portion of the hole where the cement was not in immediate contact with either the formation or a thin and hard mud cake. The mathematical analysis for this condition, as shown in the Appendix, rests on the following concepts. Pressure inside a unit length of pipe causes: (1) a tensile or tangential stress to be exerted over the longitudinal cross-sectional areas of the pipe and cement; and (2) an equal amount of strain in both the pipe and cement that is uniformly distributed over the wall thickness of each. This analysis was then used to make several calculations for a cement sheath around 51/2-in. OD pipe. The results are illustrated in Fig. 1, which shows that a tensile stress of 500 psi is imposed on a 5-in. thick sheath when the casing contains a pressure of only 1,450 psi. It also shows that a 10-in. thick sheath would be stressed to 500 psi in tension when the pipe contained a pressure of only 2,350 psi. Alternatively, if the stress analysis is made by means of the Lame thick-wall cylinder theory, the inner fibers of the 10-in. thick sheath will be stressed to 500 psi in tension when the pressure in the pipe is only 990 psi. This, of course, reveals that an unconfined sheath is of little support to the pipe in burst; however, an entirely different result is obtained when the cement is confined between the pipe and formation.

Arthur H. Elliott, New York, N. Y.: We have all been very much interested in the results of Dr. Bone's work, which Mr. Ellis has presented to us this evening. The high temperatures attained by this method perhaps afford us an explanation of the temperatures reached in the puddling-furnace with its crude and almost primitive methods of burning fuel, by means of which we have, nevertheless, been able to melt iron in a comparatively short time, and keep it in a molten condition down to a high degree of purity. No doubt many of us have wondered, as I have done, how such a result could be obtained in such a way; and it occurs to me that, perhaps, Dr. Bone has supplied the explanation in disclosing the effect on combustion of burning gas and air after passing through, and in contact with, a porous refractory body. May not the fettling of the puddling-furnace have, in some degree, an effect upon the combustion like the influence of the porous diaphragm employed by Dr. Bone ?

Jan 1, 1913

By Edward Keller

(Canal Zone Meeting, November, 1910.) UNDER the title, Labor-Saving Appliances in the Works-Laboratory, I published a paper1 in which was described how multi-manipulations, in a works-laboratory, and in the furnace-room of an assay-laboratory, can be condensed into single manipulations by applying the proper mechanical devices. For example, I now deposit in, or withdraw from, a muffle a set of 48 cupels as one unit. The front row. (8) of these. are blanks or heaters; the other 40, when they have attained the proper temperature in the muffle, are charged simultaneously with the 40 lead-buttons. Three manipulations here accomplish an operation which by the generally customary method requires 136, and this number is only limited by the size of muffle and cupels. This operation is an enlargement of what I have already described in my former paper, and Fig. I shows the improved implements. In the paper referred to I described a gold-silver bead parting-bath, which is the last of the devices used in regular sequence in practice. This bath was designated as being convenient, but was not a labor-saver properly. Fig. 2 of the present paper shows a new device. Instead of the original tray, there are now sectional holders for the test-tubes, each having a wooden handle on either end, so that the holders may be removed from the boiling bath, and the acid or water poured off from each set of tubes (in this case, 7) without waiting to cool. The tubes, held in place by clutches, as shown in Fig. 3, rest in holes in the base-strip, having a smaller diameter than the tubes. Each holder is stamped at either end with a number, so that the bath becomes further useful by permitting several men to use it at the same time without interference. Apart from the handles, the holders are made of sheet-copper. ' Trans., xxxvi., 3 to 18 (1906).

Aug 1, 1910

By J. E. Johnson

Discussion of the paper of Bradley Stoughton, presented at the Cleveland meeting, October, 1912, and printed in Bulletin No. 71, November, 1912, pp. 1245 to 1275. J. E. JOHNSON, JR., Ashland, Wis. :-Is it true that titanium reduces the chill in chilling iron? If so, as I think Mr. Stoughton has stated elsewhere, then I do not see how titanium is beneficial in car-wheel mixtures. One of the most difficult things to do is to get a proper chill and a proper degree of toughness, and the goodness of an iron of the given composition for charcoal-iron purposes is denoted by the chill which it will take as compared with its composition. If titanium reduces that chill, then it does not seem to me as good for car-wheels as its absence would be, and I should like to have it explained what effect titanium has on the chill of a given iron. MR. STOUGHTON : It is true that titanium reduces the chill of iron quite noticeably, yet, at the same time, if I am correctly informed, 90 per cent. of all chilled-iron rolls are made to-day with the titanium treatment, and a great many car-wheels, but one has to make changes in the silicon added and also, if I am correctly informed, in the manganese. The advantage of titanium is that when the proper changes are made, so that we get the same depth of chill with the titanium as we otherwise would without, the chill is much harder than before, and also the body of the roll or wheel is tougher and somewhat stronger, especially under shock. JAMES F. KEMP, New York, N. Y.:-This subject is obviously one of great importance to the iron industry, in that if we call find a method of using titaniferous ores, we will prolong the life of our iron reserves. Fifteen or more years ago, primarily from the study of the ores in the Adirondacks, I be-

Dec 1, 1912

CONTENTS PAGE Ross, J. M. and WAYLAND, R. G.-Mining Methods at the Homestake. Discussed by Benjamin F. Tillson, R. M. Raymond, I, H. Barkdoll, Arthur Notman 1 EMMEL, RUDOLPH.-Mining Methods in Zaruma District, Ecuador. Discussed by Rudolph Emmel, George A. Packard, Fred Hellmann, R. M. Raymond, Arthur Notman 2 MISHLER, R. T. and BUDROW, L. R.-Methods of Mining and Ore Estimation at Lucky Tiger Mine. Discussed by Fred Hellmann, Benjamin F. Tillson...4 PARK, JOHN FURNESS.-Mining Methods of Jarbidge District. . Discussed by R. S. Lewis : 5 Mining Methods at the Homestake Discussion of the paper of A. J. M. Ross and R. G. WAYLAND, presented at the New York Meeting, February, 1925, and issued, as Paper No. 1408-A, with MINING AND METALLURGY, February, 1925. BENJAMIN F. TILLSON, * Franklin, N. J.--It requires a good deal of timber to operate, especially the caving systems. An important function in mine operations now seems to be forestry and to operate a timber tract in order to insure a supply of timber. By depleting the timber resources of your section, you only increase your costs later when timber must be brought in from the Pacific Coast or the East. Our experience has been that any square-set method of timbering is the most expensive. Timbering for stoping systems, top slicing if you will, although it uses a large volume of time does not require as expensive timbering as the square-set method; also it does not require as long a life for-the timber, so that such wood as birch and maple, which have strength but not long life under the fungus conditions in the mine, may be used. All the drifts in the orebody are thoroughly timbered, and it has required a lot of timber. If we had it to do over, we would spend a lot more money in the development of rock drifts; as a matter of fact, we must ultimately come to that any way.

Jan 6, 1925

By W. L. DeMoulin

A rather detailed description of the entire plant and leaching process was given in a paper recently presented to the Institute,I so this paper will cover briefly only the crushing practice of the New Cornelia Copper Co. for the year 1918. The ore, which is mined by steam shovels and loaded in side-dump cars, passes through two crushing plants. These crushing plants were constructed to crush the ore required by a leaching plant of 5000 tons daily capacity, during a crushing period of 16 hours. The primary plant reduces to less than 3 in. (76 mm.) and the secondary plant, to 1/4 in. (6.35 mm.), which is sufficiently fine for satisfactory percolation of solution through the ore in the leaching tanks, and to give-good extraction. The ore is then conveyed to the leaching tanks by a system of 28-in. (71-cm.) belt conveyors. On the way to the leaching tanks, it passes through an automatic sampling plant, where a 1-per cent. sample is taken. From the primary crushing plant, the ore is conveyed by two 36-in. (91-cm.) belt conveyors to a 10,000-ton steel storage bin, with a reinforced-concrete flat bottom. The ore discharges from the bottom of this' bin onto four 20-in. belt conveyors, which deliver it to the four units of crushers in the secondary crushing plant. There is no storage bin between the mine and the primary crushing plant. The ore breaks very coarse, is very hard, and contains a great many boulders, some as large as 4 1/2 by 4 1/2 by 10 ft. (1.3 by 1.3 by 3 m.). Jams form in the bowl of the coarse crusher in the primary crushing plant, as a consequence, and are freed by means of an immense steel hook operated from a 40-ton electric traveling crane. Primary Crushing Plant The primary plant consists of one No. 24 Gates, style K, gyratory crusher, followed by four Gates No. 8, style K, gyratory crushers. All

Jan 1, 1920

By Richard A. Mullins, James J. Merle

Systematic sampling and analysis in coal-washing plants results in product control and economical operation. A well-organized laboratory system reduces operating costs and increases sales if the operating and sales companies make full use of information it supplies. The operating cost of a control laboratory is less than 1 pct per ton of coal produced. THE system of laboratory control as practiced by the Ayrshire group of mines was begun with the construction and organization of the first laboratory in conjunction with the completion of its first wash-ery in 1941. The primary purpose of this laboratory was to maintain a check on the quality of the coal produced from the washing plant. The laboratory was equipped to determine proximate analyses, float-and-sink tests, and screen analyses, and was staffed by a chemist. an assistant. and a technician. Members AIME, are Assistant Preparation Manager and Chief Chemist, respectively, Ayrshire Collieries Corp. and Subsidiaries, Danville, Ill. Joint AIME-ASME Fuels Conference. French Lick. October 1949. TP 2855 F. Discussion (2 copies) may be sent to Transactions AIME before June 30, 1950. Manuscript received Aug. 22, 1949. Soon it became apparent (1) that product control could be accomplished, (2) that a substantial reduction in operating costs could be effected by close control of coal losses in the rejects, and (3) that information furnished by the laboratory was of continuous value to the operating and sales companies. Consequently the laboratory function was expanded to supply them with additional data as required. As the parent company expanded and new mines were added, control laboratories were established at each mine equipped with washeries, and a central laboratory was maintained at one of the mines that was located equally convenient to all of them. A well-planned control laboratory assures production of a uniform, high-quality product. Whenever coal of substandard grade is loaded inadvertently, the sales company can be informed and the proper channel of distribution made. Conversely only constant and strict laboratory supervision can insure proper production of the various grades. Knowing the product, the producer can keep out of many customers' arguments that may be both awkward and expensive. Double checking between customers and mine laboratories have solved many disputes' Some nager insist On buying coal On the analysis basis only, with penalties for substandard coal and premiums for coal above normal quality. A substantial percentage of the coal sold by the Ayrshire group is of this nature. The usual procedure is for the customer to sample and analyze the coal as it is unloaded at the plant, and the mine laboratory samples it as it is loaded at the mine for subsequent analysis by the central laboratory. Only the unloaded moisture is considered, rather than the average of mine and plant moisture, and the buyer sends duplicate samples to the central mine laboratory for this determination. The average of the two analyses determines the price of coal at the mine. In this particular case, the laboratory plays an important part in increasing realization for two reasons: (1) every attempt is made to maintain plant efficiency and product quality as high as possible, (2) check on analyses and sampling by the buyer or seller.

Jan 1, 1951

By Richard A. Mullins, James J. Merle

Systematic sampling and analysis in coal-washing plants results in product control and economical operation. A well-organized laboratory system reduces operating costs and increases sales if the operating and sales companies make full use of information it supplies. The operating cost of a control laboratory is less than 1 pct per ton of coal produced. THE system of laboratory control as practiced by the Ayrshire group of mines was begun with the construction and organization of the first laboratory in conjunction with the completion of its first wash-ery in 1941. The primary purpose of this laboratory was to maintain a check on the quality of the coal produced from the washing plant. The laboratory was equipped to determine proximate analyses, float-and-sink tests, and screen analyses, and was staffed by a chemist. an assistant. and a technician. Members AIME, are Assistant Preparation Manager and Chief Chemist, respectively, Ayrshire Collieries Corp. and Subsidiaries, Danville, Ill. Joint AIME-ASME Fuels Conference. French Lick. October 1949. TP 2855 F. Discussion (2 copies) may be sent to Transactions AIME before June 30, 1950. Manuscript received Aug. 22, 1949. Soon it became apparent (1) that product control could be accomplished, (2) that a substantial reduction in operating costs could be effected by close control of coal losses in the rejects, and (3) that information furnished by the laboratory was of continuous value to the operating and sales companies. Consequently the laboratory function was expanded to supply them with additional data as required. As the parent company expanded and new mines were added, control laboratories were established at each mine equipped with washeries, and a central laboratory was maintained at one of the mines that was located equally convenient to all of them. A well-planned control laboratory assures production of a uniform, high-quality product. Whenever coal of substandard grade is loaded inadvertently, the sales company can be informed and the proper channel of distribution made. Conversely only constant and strict laboratory supervision can insure proper production of the various grades. Knowing the product, the producer can keep out of many customers' arguments that may be both awkward and expensive. Double checking between customers and mine laboratories have solved many disputes' Some nager insist On buying coal On the analysis basis only, with penalties for substandard coal and premiums for coal above normal quality. A substantial percentage of the coal sold by the Ayrshire group is of this nature. The usual procedure is for the customer to sample and analyze the coal as it is unloaded at the plant, and the mine laboratory samples it as it is loaded at the mine for subsequent analysis by the central laboratory. Only the unloaded moisture is considered, rather than the average of mine and plant moisture, and the buyer sends duplicate samples to the central mine laboratory for this determination. The average of the two analyses determines the price of coal at the mine. In this particular case, the laboratory plays an important part in increasing realization for two reasons: (1) every attempt is made to maintain plant efficiency and product quality as high as possible, (2) check on analyses and sampling by the buyer or seller.

Jan 1, 1951

By Frank H. Reed, P. W. Henline, Harold W. Jackman

A SUMMARY of the consumption of coal in 1945 shows that the coke industry accounted for 17 pct of the total coal used. No substitute for coke and the blast furnace in the reduction of iron ore has gained sufficient prominence so far to be given serious consideration. However, while the same slot-type ovens are being built and used now as were in use a few years ago, the problem of obtaining suitable coking coals, both high- and low-volatile, has forced many operators to revamp coal-blending facilities. Until the beginning of World War II, high-temperature coke plants were able to secure the required high-volatile and low-volatile coals from two or three seams and from three or four mines. Thus, many of our coke oven plants were able to operate with storage bins for two coals only. The variance in raw materials was not great, and uniformity of blend was a relatively simple problem. Since the beginning of World War II, many and important changes have taken place. Demand for all coals increased greatly. Production, though kept as near maximum capacity as possible, could not meet the demands for coal generally, and particularly for the various kinds of coal which have proved to be satisfactory for specialized uses; coals were allocated as nearly as possible in the order of greatest need; storage piling was reduced to the minimum necessary to keep plants in operation; uniformity of quality could not be maintained, and with this last, uniformity of composition of blends for coking could not be maintained. Whereas before the war producers of metallurgical coke could fill their needs from three or four mines, by the end of the war it was not unusual to find shipments to a single coke oven plant coming from as many as 30 different mines, in a single month. Since many of the mines producing both high- and low-volatile coal for high-grade metallurgical coke are rapidly nearing depletion, the problem of seeking new sources and of blending a number of coals in each plant for the production of high-temperature coke is facing practically every producer in the United States at the present time, and is one which will probably continue for many years to come. Midwestern by-product coke ovens in the Chicago and St. Louis areas use annually from 12 to 15 million tons of bituminous coals which are transported 500 to 700 miles from the Appalachian coal fields of Pennsylvania, West Virginia, and eastern Kentucky. Approximately two-thirds of this coal is high-volatile bituminous. The critical transportation problem confronting the nation in 1943, and the growing scarcity of the best Appalachian coking coals, prompted the Illinois Geological Survey to propose a research program in which would be studied the coking properties of blends of low-sulphur, high-volatile Illinois coal with the high- and low-volatile coals from the eastern fields. Such blends containing Illinois coal, if substituted for the all-eastern blends normally coked,

Jan 1, 1948

By F. Weinberg, E. H. McLaren

Dilute binary alloys have been solidified under controlled thermal conditions, and solute distributions, temperatures during freezing and melting, and the position and morphology of the solid-liquid interfaces have been examined. Binary Zn, Sn, and Pb based alloys were investigated with solute additions of AgU°, AU°, Sb'24, TlZo4, snH3, and Zns5. Approximately 150 cc of metal was used in each ingot. Appreciable solute segregation occurred in most of the ingots, depending on the solute concentrations, distribution coefficients. and freezing conditions of the alloys. Measurements were made of the general solute distribution by sectioning layers of material from the ingot circumference and counting the activity of each layer. Local segregation was detected by autoradiographic techniques. Freezing and melting curves for the same alloys were obtained by precision resistance thermometry. These curves are related to the corresponding measured solute distribution curves and those calculated from theoretical expressions. The position and morphology of solid-liquid interfaces during freezing were determined by both decanting and quenching techniques. The results indicate the manner in which freezing and remelting occurred under the conditions investigated. If an isomorphous dilute binary alloy is solidified or melted under equilibrium conditions, the concentration of solute in both solid and liquid would be uniform at all stages in the freezing process. The solute concentrations during freezing could be determined from the phase diagram of the alloy, and the freezing curves would have an alloy slope defined by the solidus and liquidus points. In practice, however, solidification under equilibrium conditions rarely, if ever, occurs, primarily because of low rates of diffusion in the solid and incomplete mixing in the liquid. As a result, the solute distribution and the shape of the freezing and melting curves obtained in a given system depends on a number of factors. These include, in addition to the extent of diffusion and mixing, the initial solute distribution and concentration, the distribution coefficient, the rate of freezing or melting, supercooling of the liquid, the morphology of the solid-liquid interface, and the effect of annealing. The purpose of the present investigation was to determine, experimentally, actual solute distributions and thermal curves for a series of dilute binary alloys, using tracer techniques to determine the solute distributions and precision resistance thermometry for the temperature measurements. In addition, observations were made of the positions and morphologies of the solid-liquid interfaces during freezing and remelting. The distribution of solute in a dilute alloy, assuming complete mixing in the liquid, and negligible diffusion in the solid, is given by1 where Co is the mean solute concentration of the alloy, C, is the solute concentration in the solidg is the fraction of the ingot solidified, and ko is the equilibrium solute distribution coefficient (assumed to be independent of concentration for dilute alloys). For the case of partial mixing, ko can be replaced by an effective distribution coefficient k. If solute transport in the liquid is assumed to be entirely due to diffusion, with negligible diffusion in the solid, then the solute distribution in the solid is given by Tiller et a1.' as where R is the rate of advance of the solid-liquid interface, D is the solute diffusion coefficient in the liquid, and x is the position of the interface from the start of freezing. The temperature at the interface TI is related to the solute concentration of the solid at the interface C, by the expression where Tm is the freezing temperature of the pure solvent and ml is the slope of the liquidus for the binary alloy being considered. Accordingly, by relating TL to the actual temperatures measured in the present experiments, solute distributions can be deduced from the temperature measurements. Using the above expressions, the measured solute distribution of a given alloy may be compared to the theoretical distributions, as well as to the distribution calculated from the observed freezing curve. EXPERIMENTAL The solvent materials used in making up the binary alloys were C. P. New Jersey zinc (99.999 pct), Vulcan Extra Pure Tin (99.999 pet), and Tadanac lead (99.998 pct). The solute elements were of 99.99 pct purity or better, and were activated in the

Jan 1, 1963

By W. A. Anderson

Recrystallization of cold-worked metals has long been known to proceed by a process of nucleation and growth.' When a cold-worked metal is heated to a temperature at which recrystallization will ensue, nuclei of new grains, essentially strain-free, appear and grow. As the process proceeds, nuclei continue to appear and to grow, until the cold-worked matrix has been entirely consumed and recrystallization has been completed (Fig. I). Conducted isothermally, a measurement of the fraction of the matrix recrystallized plotted against time, yields an isothermal recrystallization curve, showing the time course of the recrystallization process (Fig. 2).2 Evidently, then, the rate of recrystallization is determined by the rate at which nuclei form and the rate at which they grow. The rate of nucleation N is the number of nuclei that form in unit time in unit volume of the unrecrystallized matrix, and the rate of growth G is the increase in radius of the recrystallized grain per unit time. In recent years attempts have been made to determine N and G as these vary with the well-recognized variables affecting recrystallization: time, temperature, degree of deformation, etc.1 Such studies yield information that is more fundamental than that conveyed by the conventional recrystallization diagram,' since the rate of recrvstallization is thus analyzed into its two component rates3 Methods are now available by which N and G can be measured, and analytical expressions have been developed for the interrelationships among N, G, the isothermal recrystallization curve, and the final grain size, which greatly facilitate analysis.2-4 The application of these methods has been demonstrated recently for the recrystallization of silicon ferrite.2 Data on N and G in dependence upon the recognized recrystallization variables are, however, very fragmentary;" values of N and G have been determined for some metals, but the effect of temperature, which would yield the fundamentally important activation energies, has been too little studied. Thus far there has been no detailed study of the recrystallization of any one metal in terms of X and G ovcr appreciable ranges of the variables time, temperature, degree of deformation, and original grain size. It is the purpose of the present paper to provide such a study, employing aluminum.

Jan 1, 1945

By C. S. Smith, L. H. Beck

KNOWLEDGE of the Cu-Zn constitution diagram was critically examined in 1944 by G. V. Ray-nor,1 who suggested the diagram reproduced in Fig. 1 as the best evaluation of available data. No pertinent work on the constitution has been published since that time, although a number of authors have discussed transformation kinetics and theory. Despite the large amount of work that has been done on the constitution of these industrially important and scientifically interesting alloys, minor uncertainties still exist. For example, it is still not possible to say definitely whether a two-phase region exists between the ordered and disordered forms of the 8 phase. A careful re-examination of the phase boundaries in this part of the diagram was therefore undertaken. Two methods were selected for the new investigation—quantitative metallography for the higher temperatures and precision lattice parameter measurement for lower temperatures. Because of the relatively narrow two-phase regions flanking the ß phase in these alloys, quantitative metallography is particularly suited for their examination, since the relative amounts of the two phases are very sensitive to their compositions. The method, however, is useless below about 350°C because of the inadequate resolution of the two constituents. Below 400°, however, the X-ray diffraction method is applicable, although it is of somewhat lower sensitivity in this system. The changes of composition that occur during quenching from above about 500°C entirely vitiate X-ray measurements at room temperature though they do not affect metallographic area measurements. The two methods overlap and supplement each other admirably. Both methods depend on the attainment of equilibrium composition of the two phases in a more or less intimate mixture and thus avoid the difficult problems of nucleation and long range diffusion involved in the conventional metallographic bracketing method. The alloys were melted from a master alloy made from re-electrolyzed cathode copper and Horsehead 99.99 pct Zn. Melting was done under a cover of either borax or charcoal and the alloys cast into a 7/8 in. sq graphite mold for the a-ß alloys or a 3/8 in. diam cylindrical graphite mold for the ß-? alloys. The a-ß alloys were rolled at 750°C to 5/8 in. sq; annealed for 24 hr at 800°C and quenched; then rolled and swaged at 200°C to 3/8 in. diam rods, annealed 24 hr at 200°C, quenched and cold rolled 2 pct reduction. This treatment was intended to obtain a small grain size and to produce many nuclei of the minor phase for growth on subsequent heat treatment. The unworkable ß-? alloys were given preliminary treatment by sealing in Vycor tubes in vacuum and annealing for 4 hr at 800°C followed by cooling in air. Samples of homogenized alloys were checked spectrographically for impurities, but the principal components were determined on samples subsequent to heat treatment. The impurities analyzed averaged approximately as follows: Ag, 0.0002 pct; Fe, 0.004; Si, 0.0008; Cd, 0.005; Mg, 0.0002; and Pb, 0.002. For metallography, samples of appropriate composition were cut into rods 5/8 in. long, sealed in pyrex tubes in vacuum and annealed for eight weeks at temperatures of 470°C and below, two weeks at 480°, 500°, and 600°C, and 4 hr at 700°C, followed by quenching in cold water. Temperatures were accurate to ±2°C. The cylinders were then machined to 8.7 mm diam and a slice weighing 1.5 g cut with a thin saw transversely from the center of each. This

Jan 1, 1953

By Strathmore R. B. Cooke

On the basis of experiments conducted on quartz using a bubble pick-up method, it was shown in an earlier paper1 that this mineral will preferentially adsorb hydrogen, calcium, or sodium ions, depending on the relative concentrations of those ions in the solution in which the quartz is immersed. For quartz particles ranging in size from 0.2 to 1 mm, it was demonstrated that the concentration of calcium in solution (assumed present as ions) necessary to completely activate quartz for flotation is given by the expression: Ca++ = [H+] X 106 + [Na+] X 10-3 In this expression, ionic concentrations are in mols per liter. It was further shown that the pick-up method is apparently more sensitive to changes in reagent concentration than the standard captive-bubble method, and that induction times are apparently much reduced. Since completing these earlier tests, a new type of cell has been constructed; this is shown in Fig 1 and 2. In Fig 1, A is a ground joint, B is a central tube reaching to within a few millimeters of the bottom of the cell, and C is a stopper which may be removed for reagent addition, and serves the further purpose of excluding carbon dioxide from the air during the test. The entire cell is constructed of Pyrex glass, and does not give the trouble experienced with the earlier cell, in which activating ions were released from the glass at high pH values. The only critical factor in the construction of the cell is the clearance between the central tube and the bottom of the cell. This clearance should be sufficiently small that the bubble can be pressed directly on the mineral grains lying on the bottom of the cell. In the pick-up tests to be described in this paper, the reagents used were all of C. P. grade, except the sodium oleate, which was Merck's "neutral powder." The quartz employed was water-clear vein quartz, sized on screens, cleaned with both hydrochloric acid and sodium hydroxide, and given a thorough final washing with distilled water. Experimental procedures were the same as described in the earlier paper. EFFECT OF SIZE OF QUARTZ ON PICK-UP To ascertain the effect of particle size on the adsorption of calcium ions, the quartz was sized from minus 14 plus 20 mesh through the intervening screen sizes to minus 270 mesh plus 400 mesh. Each size was thoroughly cleaned, and then tested in the cell at different calcium chloride and sodium hydroxide concentrations, and at a constant sodium oleate concentration of 20 mg per liter. All particles, within the size range given, exhibited complete pick-up within the curve expressed by the equation above. This presumably means, when the conditions imposed by the equation are satisfied, that this maximum is independent of particle size. However, it was found that the range through which partial particle pick-up occurred progressively broadened as particle size decreased. This is shown in Fig 3, in which curves B, C, and D show the limits at which pick-up just commences (as the pH is increased) for particles of minus 14 plus 28 mesh, minus 65 plus 100 mesh, and minus 270 plus 400 mesh size, respectively. These results indicate that for satisfactory activation, at any given pH, a lower calcium ion concentration is required for fine particles than for coarse particles. EFFECT OF HIGH ALKALINITY ON PICK-UP At calcium concentrations of between 1 and 10 mg per liter, and at high alka-linities, it was noticed that pick-up ceased as soon as calcium hydroxide commenced to precipitate. This effect was investigated at other calcium concentrations, with the same results. Solutions of calcium chloride, containing 105, 104, l03, and l02 mg of calcium per liter were made alkaline with sodium hydroxide until calcium hydroxide just started to precipitate, according to the following equation: CaCl² + NaOH -+ Ca(OH)2 + 2NaCl The beginning of precipitation was taken as that point at which either a faint opalescence appeared in the solution, or a Tyndall cone became ap-

Jan 1, 1950

Prof. Henry M Howe, New York: It is extremely probable that this efflorescence of silica is due to the liquation either of silicon or of a silicide, and the subsequent oxidation of the silicon to silica. As Mr. Fackenthal says, it is very hard to see why silicon should liquate from an iron containing so little silicon, and it seems more probable that some silicide of some volatile element has liquated, and has dissociated on reaching the air, and that the volatile element has volatilized, leaving the silicon to oxidize to silica. The volatile elements present which might thus liquate in combination with the silicon are sulphur, zinc, and lead. It is hard to see why sulphide of silicon should have liquated from an iron containing so little of either sulphur or silicon. At first, one naturally thinks that either the zinc or the lead present in this furnace might have liquated as silicide. It is true that they are both volatile at the temperature within the furnace, but then the vapor-tension* of each of them within

Jan 1, 1901

By J. A. Hren, G. Thomas

A high-temperature stage has been used to study precipitation and dissolution in thin foils of Al-20pct Ag alloy directly in the electron microscope. The results show that the aging characteristics are similar to those observed for bulk materials, and in addition, direct evidence is presented for clustering at the solid solution temperature. The limit of solubility of G. P. zones is-350°C. The heterogeneous precipitation, the growth and dissolution of ?&apos;have been studied in detail. Growth of ?&apos; parallel to the basal planes, occurs by continuous motion of inter -facial partial dislocations. Growth stops at intersecting particles due to formation of sessile a/6 <110> interfacial dislocations. Growth normal to the habit plane occurs by the spontaneous nucleation of partial dislocations on alternate (111) planes and the thickening rate is --10-3= times the lengthening rate. The precipitates dissolve in layers and the final product is a whole a/2 <110> dislocation . The nucleation -growth -dissolution processes are thus completely reversible. Kinetic data obtained from the dissolution rates of ?&apos;particles enable the diffusion coefficient to be determined and the activation energy is found to be 37.5(±4) kcal mol-1, which is that expected for dzffusion of silver in aluminum. The velocity of the interfacial dislocations is thus dependent solely on the rate of diffusion of silver atoms. RECENTLY it was demonstrated that a high-temperature stage could be effectively used in the electron microscope to follow directly the processes of precipitation and dissolution in thin foils of A1-4 pct Cu alloy.&apos; These experiments also provided kinetic data which enabled the diffusion coefficient to be estimated. This new development of electron metallography opens up many fruitful areas of research and it was decided to investigate the aging behavior in thin foils of A1-20 pct Ag alloy, particularly the mechanism of heterogeneous precipitation (i.e., precipitation on lattice defects). This system was chosen because the aging characteristics of bulk specimens are now well known,2"7 and because we wished to obtain more details of the role played by partial dislocations and stacking faults in the nucleation growth and dissolution of the hcp ?&apos; phase. This is of interest for the general case of fcc-- hcp transformations. Part of the A1-Ag phase diagram is shown in Fig. 1. The use of a high-temperature stage also enables a study to be made of the clustering process (formation of G. P. zones) and to determine the structure of the solid solution prior to the usual quenching and aging procedures. It is also possible to obtain kinetic data from measurements of the rates of dissolution of precipitate particles. Unlike the results of previous experiments on A1-4 pct CU 1 where much of the initial precipitation occurred on the foil surfaces, the results on the A1-20 pct A1 alloy were identical to those reported for bulk specimens6,7 and no surface precipitation was ever observed. Thus, it was possible to follow the aging sequence: G.P. zones — ?&apos; — ? directly in the thin foils. This paper is concerned with the formation and dissolution of zones and the ?&apos; phase, and no attempt has been made so far to follow the mode of discontinuous precipitation of ?. I) EXPERIMENTAL DETAILS The high-purity A1-20 pct Ag alloy was prepared by the Aluminum Co. of America in the form of 0.001-in.-thick sheets. These were cold rolled with intermediate anneals to a thickness of 0.0004 in.,

Jan 1, 1963