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By S. Senderoff, D. E. Couch

A PROCESS for the electrolytic preparation of molybdenum from molten salts has been described previously. This previous work centered on electrowinning and electroplating characteristics of the process. In this paper the properties of the process as a refining medium are discussed. In producing metals from ores, it frequently has proven most economical to obtain a comparatively impure metal by smelting, and to purify the product by electro refining. Direct electrowinning from molten salts is rather difficult when a porous diaphragm is required in the process, as in the case of molybdenum, since satisfactory refractory materials for such a diaphragm in molten salts have not yet been developed. In electrorefining, however, a soluble anode is used. By suitable control of anode and cathode current densities, the lower-valent molybdenum compound used in the electrolyte is not oxidized, and a diaphragm is not needed, thus avoiding difficulties which are encountered with other electrowinning processes. Electrorefining may result from two different processes in the cell: Dissolution of the molybdenum and the less noble impurities with a separation of the more noble impurities as an anode sludge; the electrodeposition of molybdenum and the more noble metals at the cathode, leaving the less noble metals in the electrolyte. The amount of separation which occurs in each process is determined by the potential of the operating electrode and the relative concentration of the various species at (or in) that electrode. Since molybdenum has a comparatively noble position in the EMF series in molten alkali halides,2 most refining would be expected to occur at the cathode. In this work only the cathodic process was studied. The objective was to determine to what extent various metallic ions, if they dissolve from the anode or are otherwise introduced, were concentrated in the electrolyte. The necessary conditions for the separation of each and the limiting concentration which may be tolerated in the electrolyte for effective refining were studied. The deposits were chipped from the cathode and analyzed spectrochemically for metallic impurities. Besides determining the major contaminant, a general qualitative analysis was obtained to be sure that other metallic ions were kept at a very low level during each series of runs and to be sure that the baths were not being contaminated accidentally. Samples of the bath, for analysis, were taken at the temperature of operation so there was no chance of selective crystallization during cooling. In this way the ratio of molybdenum in the bath to the other metal could be determined readily. These data permitted a check on the anode efficiency and any volatilization that took place during the electrolysis. Experimental Apparatus—The apparatus as shown in Fig. 1 was used to determine the effect of the various foreign ions upon electrodeposited molybdenum. The entry chamber A allowed the cathodes to be removed without cooling the bath and without allowing oxygen or moisture to enter." The cathodes were made Prom 0.25-in. tungsten rods and were rotated during the electrolysis. The balloon in the lower arm B was inflated with helium after the cathode was drawn up into the upper section for removal. A new cathode was then placed into the entrance chamber A after which the chamber was flushed

Jan 1, 1959

By Myron Rodgers

IN rock- or ore-crushing tests all data, in order to be valuable for study and comparison, should be obtained and tabulated under conditions as uniform as possible. The results of many such tests have no value for comparison, because of incomplete data and the lack of uniform conditions, screens and scale of sizing, etc. The purpose of this paper is to suggest a form of standard specifications which may be developed by the Milling Committee and approved by the A. I. M. E. for rock-crushing tests. It is not intended to discuss any theories of rock crushing. Reports of rock-crushing tests should include the following details: 1. Description of the machine employed (jaw or gyratory crushers, rolls, stamps, tube mills, Chilean mills, etc.). 2. Method and material (timber, concrete, etc.) of foundation. Much power is dissipated in the vibration of poor foundations. 3. Locality from which the rock or ore was obtained, and geological, mineralogical, and physical characters of the material. 4. The power consumption of the machine running with no load and with full load, the unit of power being 1 hp, per 24 hr. 5. The capacity of the machine in tons (of 2000 lb.) per 24 hr. 6. The duty in tons per horsepower-day. 7. The screen analysis of feed and product by the proposed A. I. M. E. standard screen scale. On the foregoing statement, the following remarks are offered.

Jan 9, 1915

By Francois E. Heuze

The Crestmore Mine of the American Cement Company lies at the eastern end of the Jurupa Mountains, 50 miles east of Los Angeles. Originally, a quarry was opened in 1908 for "limestone" used in the manufacture of cement. The mining operations eventually went underground employing first a modified system of block caving and later the "room and pillar" scheme. The limestones are relatively small roof pendants preserved in an enveloping and intrusive quartz diorite. They occur as two irregular lenticular bodies roughly parallel at the top and tending towards convergence at depth. Their dip varies between 25 and 30 degrees E. The presently mined lower bed, Chino limestone, is typically composed of alternating bands a few inches to a few feet thick of medium to coarsely granular white crystalline limestone and somewhat yellowish limestone (brucite marble). A "room and pillar" scheme of mining is currently employed in the lower body of the Crestmore Mine. The levels are horizontal and access is provided by a spiraling road starting in the old quarry. The present depth of operations is an average 750 ft below the surface. Fig. 1 gives a three-dimensional general sketch of the mine. The long axis of the rooms is in an E-W direction, normal to the strike of the beds. Fig. 2 is a horizontal map of the 130 level, the deepest level mined presently. It is in this level that most of the in-situ investigations have been conducted. The present investigation was made possible by a non-restrictive grant of the American Cement Company to the University of California. The program included a series of in-situ tests using flat-jacks, plate bearing,

Jan 1, 1968

By Leon W. Dupuy

Many articles have been written describing peculiar and particular types of drilling. Little correlation has been made between the character of ground to be drilled and sampled and the type of drilling most desirable for procuring satisfactory samples. In development work, the engineer and metallurgist often desire the recovery of a sample in as physically natural a condition as possible, particularly when the sample must provide material for process tests as well as chemical and physical analyses. This paper describes the results of experimentation in drilling unconsoli-dated materials carrying titanium minerals in the Magnet Cove area, Ark. The drilling was most difficult in that the ground varied much in consistency, and it was vitally necessary to recover a physically natural sample. Ordinary churn drilling recovered a sample that could be analyzed chemically, but the sample was not in its natural state. The problem was successfully solved by utilizing and further developing methods used in the oil and clay industries. In the Magnet Cove area of Hot Spring County, Ark., the titanium minerals include rutile, brookite, ana- tase, leucoxene, and others. They occur in soil, clays, and altered rocks adjacent to novaculite in contact meta-morphic deposits. In preparing titanium minerals for use in the industry, it is necessary to know the physical characteristics of the ore. Also it is believed that the particular physical character of the titanium mineral used is just as important as the chemical character. Brookite and rutile, for example, are the same chemically but differ in crystalline structure. In preparing titanium minerals for market, beneficia-tion is necessary. For the millman to make a satisfactory laboratory test, the sample he uses must be as nearly of the same physical character as he would have from mine run ore. In the past at Magnet Cove, churn drilling had been done on the properties, and assays of total titania had been obtained. It was found, however, that the total titania was indicative merely of the presence of titania but did not tell the metallurgist the character of the material or even give him the slightest indication of what he might expect to recover. When the Bureau of Mines entered the field in the winter of 1947 and 1948, it was therefore necessary that a natural sample be recovered. LIMITATlONS IN ORDINARY PRACTICE The churn drilling that had previously been done had shown that the occurrence of titanium-bearing mineral was somewhat widespread. The samples were, however, completely beaten up and in a finely powdered state. The minerals had been slimed, and such ore dressing tests as were made from the churn-drill samples were found to be worthless. Test pitting and outcrop sampling had provided satisfactory samples of surface ore but did not represent the entire ore body. A quantity of rutile had been produced from the surface residual concentrations in the westerly part of the cove, but production ran into metallurgical trouble as depth was attained. Representative deep samples upon which ore dressing research might depend were needed.

Jan 1, 1950

By H. S. Drinker

THE first discovery of zinc 011 the property now worked by this company was made by the celebrated mineralogist, Prof. William Theodore Rapper, in 1845. Different claimants kept the property in continual litigation till 1861, when everything was satisfactorily settled by the purchase of the land by the company, who have worked it ever since. The mines are situated in a valley, four miles south of Bethlehem, Pa., in Lehigh County. The valley is from two to three miles broad, and is bounded 011 the north and south by syenitic hills. Syenite underlies the valley, and upon this is deposited the Potsdam sandstone, then a layer of slate, and, finally, a dolomitic limestone, belonging to the Chazy or Black River formation, in which the zinc deposits are inclosed. The rocks occur in folds, and have evidently been subjected to tremendous pressure from below, the zinc deposit being found in an anticlinal axis, in nearly vertical veins. I t is supposed that the zinc was originally disseminated through the

By V. R. Garflas, J. W. Ristori, R. V. Whetshel

Preliminary estimates indicate that world consumption of petroleum products and related fuels in 1937 shattered previous records with a figure of 1,920,000,000 bbl.; that is, 124,000,000 bbl. more than the 1936 total. The writers, as in previous years, have been unable to account for all the available supply in 1937. This "unaccounted-for" supply, which formerly was thought to go largely into storage in foreign countries, was close to 53,000,000 bbl. in 1933; 93,000,000 in 1934; 111,000,000 in 1935; 75,000,000 in 1936 and 148,000,000 in 1937. As this discrepancy between supply and demand continued year after year, it became evident that other reasons than additional foreign stocks were responsible for it. It can now be stated that the "unaccounted-for" supply (see Table 1) goes to take care of: (1) consumption of petroleum products and related fuels for military purposes, the figures of which have been and are kept confidential by foreign countries, (2) additions to stocks to be consumed for military and nonmilitary purposes in foreign countries on which likewise no information is available, (3) errors incurred in the conversion of figures of production of crude oil, its products and related fuels from "weight" units, as used in Russia, for instance, to their American or "volume" equivalents and vice versa, and (4) to the lack of reliable statistics on production and consumption, particularly from Russia, the

Jan 1, 1938

By F. Keller

ALUMINUM alloys containing magnesium and silicon are susceptible to strengthening and hardening by suitable heat-treatments, and they constitute a class of alloys of considerable commercial importance. Generally, they contain these two elements in the proportions required for the formation of the intermetallic compound Mg2Si, or an excess of silicon; no commercial wrought alloys are made with an appreciable excess of magnesium. The reason for not having excess magnesium is obvious from the results given in this paper, since it is shown that excess magnesium results in a proportional decrease in the solubility of Mg2Si. This is the eighteenth1 of a series of papers from the Aluminum Research Laboratories dealing with the equilibrium relations in aluminum-alloy systems; most of the previous publications concerned binary aluminum-alloy systems; this is the fourth of a group pertaining to ternary aluminum-alloy systems. The work on this system was com-pleted in 1930, but the results were not published because of the pressure of other work. Hanson and Gaylor2, in 1921, presented the results of an extensive investigation of the aluminum-magnesium-silicon system. Their results indicated that an excess of magnesium over the amount required to form the compound Mg2Si caused a noticeable decrease in the solid solubility of Mg2Si in aluminum. A more recent investigation3 in these laboratories showed that the solid solubility of Mg2Si in aluminum was 1.85 per cent at 595° C. and decreased to 0.30 per cent at 300° C. The results of the latter investigation were used as the basis for the present work.

Jan 1, 1936

By Samuel Lasky

WITH the movement of American capital into foreign investment, a new field of specialization for the American mining engineer is gradually opening a field hitherto entered almost wholly by chance and without full appreciation of its possibilities. Our age has been fitly called the "Age of Specialization." The special application of one's knowledge and ability to a definite and restricted branch of .his profession is purely a modern condition. Any profession, or branch of a profession or, industry, in which the problems may be segregated into definite types, calls for specializa-tion. Modern industry demands efficiency and that, reduction and ultimate annihilation of waste. Effort and time wasted by workers' on a problem with which they are not familiar is as flagrant a waste of money -the final standard-as any waste of materials. One of the subdivisions of mining engineering which is beginning to be recognized is of engineers who are clearly conversant with the particular and peculiar problems obtaining under foreign operating conditions. The need is as yet obscured, however, by the domestic prosperity of our American mining industry. The opportunity here lies more with the American engineer than with other nationals. The foreign en-gineer now in that service is not there through a realiza-tion of the special opportunities that exist, but through necessity, whereas, with the American engineer, more especially ,the recent graduate or those who will soon graduate, this is a new field to be entered wholly by choice. As a matter of fact, many engineering students will find it necessary to seek foreign service if they wish to remain in mining. Although the scope of the domes-tic industry is tremendous and there are many positions open to the junior engineer, there are not enough for the great number of graduates turned out yearly from our, mining schools. Educators tell us that less than 40 per cent. of the students in engineering schools gradu-ate; and of these but a minority continue in engineering. Even this minority is too great for our domestic. In-dustry, and although the young engineer realizes that condition after a few years he rarely seeks foreign work. A. perusal of the directory of the American Institute of Mining Engineers indicates that, but about one-half of one per cent of the Junior Associates are in positions outside of North America. Granting that most of them are still in school, the figure is surpris-ingly small.

Jan 1, 1927

By Richard D. Call

Predicting the performance of a waste embankment requires an estimate of the properties of the waste and foundation materials. The performance characteristics and the associated material properties are: [ ] Methods for obtaining estimates of the material properties include: laboratory and field testing, back analysis, and indirect estimates from other material properties. The most critical technical need is the development of indirect methods for use in feasibility studies and mine planning, prior to production when actual samples of waste material are not available. Material properties are not unique, single values; they are probability distributions. There are two components to these distributions: the uncertainties in testing and the inherent variability of the material. The objectives of a material properties evaluation should be to obtain an unbiased estimate of the property distributions rather than the average or the minimum value. Whether the current trend to a probability design analysis is followed or a simple sensitivity analysis is conducted, the unbiased probability distribution is preferable to single values.

Jan 1, 1985

By D. F. Hewett

ALTHOUGH most persons will agree that an individual or a nation can profit from the experience of other individuals or nations, there is always room for debate over the degree of similarity of their past and present conditions and of their future problems. Noting the increasing interest that Americans are showing in our mineral problems, I have felt that we could profit from reviews of the experiences in mineral exploitation acquired by the industrial nations of Europe. Whether we can learn much from Europe's experience in exploiting such minerals as petroleum may be debatable, but certainly, with a record of metal production extending back nearly 3000 years, Europe should hold much of value for America. A trip to Europe in 1926 permitted me to visit 28 mining districts, of which about half are now or have been in times past outstanding sources of several metals. The districts range from England to Greece and from Spain to Poland. To summarize briefly my impressions of these mining districts, as well as such reactions to the thought and life of Europe as so short a visit permits, I shall only venture the opinion that Americans can review with great profit the ideas and actions of Europeans, with regard not only to the production of metals but to many expressions of life. I believe that America has made and is making new contributions to the art of living, as well as to the arts of mining and metallurgy, but in so far as Europe is and has been a laboratory of economic, social and political experiments, the results she has attained deserve the thoughtful attention of America. I have come to believe that many of the problems that harass Europe lie in our path not far ahead. I have therefore hoped that a review of metal production in Europe in the light of its geologic, economic and political background may -serve to clear our vision with regard to our own metal production.

Jan 1, 1929

By Norman Weiss

THE need for more efficient utilization of labor in the metal-mining industry has been the subject of several recent editorials in the mining press, and one attractive possibility for such improvement lies in the designing of future milling plants particularly with economy of man-power in mind. We are accustomed to think of mill design as the selection and coordinated arrangement of process equipment, but if labor is to be efficiently utilized it must be given early consideration in planning the new mill. There are three good reasons for economizing in labor: (I) to reduce costs, not only in the form of wages but also in housing, hospital, welfare, and other obligations that a company accepts when a new man is added to the payroll; (2) to prepare for recurrent periods of manpower shortage, during which a well-designed plant can manage to get along with skeleton crews; (3) because a milling plant that must depend upon an inordinately large labor force for its operation and maintenance is certain to be inefficient in other respects, for many of the shortcomings in design that make necessary the excessive use of labor are generally not corrected merely by having too many men. A simple example of this is a poorly designed ore-feeding system: if this is inadequate to the extent that one man must be constantly unclogging feed chutes, it may help the situation to put two men or three at this task instead of one, but the feed rate will still be inconstant. First of the factors that affect labor saving is the location of the mill. This is often determined by transportation costs alone, and as a result the mill may be placed close to the mine regardless of the nature of the terrain. The designer must then adapt his layout to the conditions, favorable or not. This happens often at small properties, where capital investment may seem more important than operating expense. In most instances, however, a mill site carefully selected for the advantages it gives the designer in laying out the plant is the most economical in the long run, even if it involves a slight increase in cost of ore haulage. Given some freedom of choice, the design engineer may be able to find just the piece of ground that provides the proper gradient for the needs of the flowsheet, permits installation of essential yards and trackage, and perhaps supplies an excellent site for a tailing dam. Further justification for having placed the mill not too close to the mine sometimes emerges only years later as an opportunity to treat ores from other properties. When it is known from the beginning that the new mill will serve a number of scattered mines, a free choice of mill site is naturally stimulated. The most important single factor in limiting the labor requirements of a mill is its materials-handling system for bring-

Jan 1, 1946

By G. H. Gronhovd, W. H. Oppelt

Complete gasification to produce synthesis gas for manufacture of synthetic chemicals and fuels offers possibilities for utilization of the vast lignite fuel deposits in the U.S. The design of a slugging, fixed-bed, pressure gasification pilot Plant is described. Results are presented for initial operation of the plant at moderate pressure and using low-temperature char as fuel. Gasification of solid fuels is becoming increasingly important in the future overall energy picture, both in this country and abroad. Snythesis gas from gasification of coal consists chiefly of carbon monoxide and hydrogen, and after suitable purification and modification this gas can be used in the production of synthetic ammonia, methanol, higher alcohols, and synthetic liquid fuels, or as a reducing gas in the metallurgical field.' Most synthesis gas used in this country is made from natural gas, petroleum oils, and refining tail-gases, but the direct gasification of coal will become more attractive as costs of petroleum oils and natural gas increase.' A gasification process designed for use with brown coal and lignite was developed by the German Lurgi Co. prior to World War 11. In this process a fixed bed of lump-sized fuel is gasified with steam and oxygen at pressures ranging from 370 to 440 psi. Effective heat exchange between the ascending high-temperature gases and the descending solid fuel results in low gas outlet temperatures, high thermal efficiency, and favorable oxygen consumption. Lurgi gasifiers are used commercially for the production of synthesis gas or as a substitute for coal gas in many countries, including Germany, Czechslovakia, Great Britain, South Africa, Australia and Pakistan.3-6 The chief disadvantage of the conventional Lurgi gasifier which operates under nonclinkering conditions is that large quantities of excess steam must be supplied with the oxygen-steam mixture to reduce the temperature in the fuel bed below fusion temperature of the ash. Most of the steam leaves the gasifier undecomposed with the product gas and, after cooling, produces large amounts of dilute liquor. Evaluation of fixed-bed gasification experiments using dry-ash removal indicated that by increasing the oxygen concentration in the oxygen-steam blast the temperature in the combustion zone could be raised high enough to operate under slagging conditions. 7-8 Operation of a fixed-bed pressure gasifier under slagging conditions would reduce the steam requirements and the volume of waste liquor and would increase the steam decomposition, the overall thermal efficiency of the process, and the rate of gas production per unit cross sectional area of the gasifier. Because the Lurgi gasification process, modified for slagging operation, offered possibilities for efficient gasification of American lignite, the Bureau of Mines decided to investigate the process on a pilot-plant scale at the Grand Forks, N. D., Lignite Research Laboratory. DESIGN Description of Pilot Plant: A flowsheet of the Grand Forks slagging gasification pilot plant is presented in Fig. 1. The gasifier unit consits of the coal lock, the gas generator, and the slag lock. The fuel, which is periodically charged to the coal lock, moves by gravity flow into the generator and is continuously gasified by an oxygen-steam mixture introduced at the bottom of the gasifier. Molten slag is formed at the hearth and flows through a central taphole into a water quench bath. The slag-water slurry is periodically discharged from the slag lock. Process steam is generated and superheated in separately-fired, oil-burning units. Oxygen is supplied to the gasifier from a gas storage bank located some distance from the pilot plant. The capacity of the oxygen storage bank is about 130,000 standard cu ft at 2200 psig. Liquid oxygen is delivered by truck and is converted to gas during the filling operation. The superheated steam and oxygen are metered separately, then mixed and fed to the gasifier tuyeres. The gas generator is surrounded by a water jacket. The steam formed is separated in the steam drum and then discharged to the gas offtake, thus equaliz-

Jan 1, 1961

By T. L. Fritzlen

EXTRUSION of aluminum alloys in this country is performed mainly by direct extrusion, therefore this paper is confined only to factors affecting the rate of extrusion by this method. Many factors affect the rate of extrusion of aluminum alloys. It is the purpose of this paper to present a discussion on the factors that are subject to technical control. Most of them are closely related, so that a clear-cut distinction between them is rather difficult. However, an attempt will be made to evaluate the effect of each factor separately, as far as possible. The most important factors only will be considered, and these will be discussed in detail under three general headings: (I) characteristics of the equipment, (2) size and structure of the ingot, and (3) temperature of ingot, cylinder, and other parts. It is a well established fact' that the pressure and the speed of extrusion are related and are exponential functions of one another. Therefore, whenever a certain condition tends, for instance, to increase the pressure required for extrusion, it will reduce the extrusion speed if the pressure is maintained constant. For this reason, in this paper the effect of various conditions is expressed either in regard to their effect on the pressure required or the extrusion speed. Another established fact is the relationship between the temperature of the material being extruded and the pressure required to extrude. According to Schishokin,2 this relationship is of the exponential type, and as the temperature is increased the pressure required is decreased. It would seem from the preceding that the greatest rates of extrusion can be obtained by the use of higher temperatures. However, as is well known, other factors intervene to limit the rate of extrusion of aluminum alloys when increasing the temperature. These factors will be discussed in detail later. CHARACTERISTICS OF THE EQUIPMENT The capacity of the press determines the maximum unitary pressure that can be applied for any given cylinder diameter. Pressures used for extrusion of aluminum alloys range from approximately 50,000 lb. per sq. in. to 150,000 lb. per sq. in., dependent upon the alloy and the size of the shape extruded. Higher pressures could be used to advantage, but existing steels limit pressures employed in the production of extrusions. Numerous mechanical characteristics of the extrusion press affect extrusion rate. The most important characteristics of the press itself are: (I) sensitivity of the main pressure valve and accuracy of pressure gauges, (2) accuracy of equipment to heat the cylinder uniformly and to control cylinder temperature, and (3) accuracy of means of measuring the speed of extrusion. The variables subject to control during the extrusion operation are pressure, temperature, and speed, and it is evident that the preceding characteristics

Jan 1, 1945

THE education of adolescents to perform the duties and assume the responsibilities of maturity has been a characteristic of human society since the dawn of history. In the beginning the members of the immediate family performed this function, and in modern life they still have an important part in it. Possibly religion was the first field in which education began to be functional; young people were sent for instruction to a teacher who had a broader and deeper knowledge of the subject than was possessed by the family. It does not seem necessary for our purpose to attempt to determine how, when, or where instruction in the practical arts first began to become functional, and the brief outline which follows must suffice. The discovery and utilization of mineral substances to improve and maintain the conditions of human living is a practical art, which must have had an almost accidental origin and have been developed by empirical experiments. We do not know, nor would it be useful to try to fancy, how men first learned that they could make use of mineral substances to their benefit, but however that knowledge was initially gained it was certainly trans- mitted through instruction in the family. At fist such activities must have been merely a minor part of the making of a living, bit in time those who excelled found it better to devote them-

Jan 1, 1941

By Thomas M. Drown

THE means relied on to attain uniformity in Bessemer steel may be enumerated as follows I. The appearance of the flame. II. The appearance of the slag. III. The spectrum of the flame. IV. Examination of the steel itself. At present, I wish briefly to bring forward a few considerations with reference to the last two mentioned, namely, the conditions favoring the employment of the spectroscope and examination of the steel. From the amount of careful investigation which has been devoted to the examination of the Bessemer flame by the spectroscope, both on the part of scientists and practical metallurgists, one might reasonably expect some results definite and satisfactory in their nature, first, as regards the nature of the flame, and second, as to the practical value of the spectroscope as a guide in conducting the process. We find, in fact, however, that uncertainty and confusion still exist. In Germany, where this subject has received the greatest attention, it is now very generally conceded that manganese is the cause of the well-known groups of dark bands that characterize the Bessemer spectrum. Nor is it easy to see how we can avoid accepting this conclusion, when Wedding and Von Lichtenfels have produced the manganese spectrum and found it to correspond closely with that shown by the Bessemer flame. But it is evident, on a moment's reflection, as Roscoe has recently brought forward, that manganese cannot be the only cause of the Bessemer spectrum, for we notice the characteristic bands quite as

Jan 1, 1873

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

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Jan 1, 1938

By John D. Roach

DURING an investigation of the yttrium-hydrogen system aimed at producing solid yttrium hydride specimens containing various amounts of hydrogen, it was observed that yttrium containing approximately 2 wt pct H exhibited a tendency to crack and crumble to a powder on standing in air at room temperature. It was also observed that longer hydriding times, at a given temperature, increased this susceptibility to powdering without an increase in hydrogen content, also that moisture in the air is necessary for the observed effects to occur. Even if cracking did not occur, there was a continual formation of a light gray powder on the as-treated surface of the hydrided yttrium and this reaction continues until the entire hydrided piece has been reduced to a powder. Storing the hydrided specimens in the absence of air or removing the surface either by machining or grinding were effective means of preventing this disintegration of hydrided yttrium. In an attempt to determine the reason for this powdering phenomenon, the surfaces of a number of as-hydrided yttrium specimens were examined by X-ray techniques. In all cases the X-ray pattern obtained showed the major phase to be yttrium hydride (YH2) as would be expected since the specimens contained 2 to 2.2 wt pct H. In some cases a trace of yttrium oxide was observed. There was also a third phase present on the surface of these hydrided specimens which could not immediately be identified. This unknown phase was a face-centered cubic material, NaC1-type structure, with a lattice parameter of 4.855 and a calculated density of 5.914 g per cc. Very slight hand polishing of the surface of the hydrided yttrium specimens completely removed both the unknown phase and the traces of oxide so that only the yttrium hydride pattern remained. Based on the X-ray patterns the quantity of the unknown phase on the surface of the hydrided yttrium appeared to be directly related to the susceptibility of the material to powdering. Work at the Denver Research Institute on the yttrium-nitrogen binary system showed that yttrium nitride (YN) is a face-centered cubic material with a lattice parameter of 4.878A and a density of 5.890 g per cc. They also noted that this compound rapidly disintegrated to a powder on standing in air. The unknown pattern observed in the above specimens corresponds very closely to that of the nitride—fcc structure, 4.885 parameter, and density of 5.914 g per cc. The presence of this thin film of nitride on the surface of the hydrided specimens probably accounts for the observed powder formation and crumbling. The nitride reacts with the water vapor in the air (verified by private communication from Dr. C. Huffine, General Electric Co.) to yield yttrium oxide and ammonia. Ammonia is readily detected when hydrided yttrium specimens were allowed to stand in bottled moist air. The powder formed on the surface of the hydrided specimens was shown by X-ray analysis to be yttrium oxide. This reaction appears to occur primarily at the grain boundaries since discrete particles of yttrium hydride separate from the specimens during this powdering process. The reaction of yttrium nitride with water vapor is believed to be as follows: 2YN + 3H2O - Y203 + 2NH3. Despite the fact that this nitride is present only as an extremely thin surface film, if the above reaction is not prevented by removing this film from the surface either by machining or grinding, the reaction continues until the entire hydrided piece has been reduced to a powder. To account for this continuation of the reaction, it is believed that the following reactionalsooccurs: 2YH2 + 2NH3 -2YN + 5H2. The nitride produced by the latter reaction reacts in turn with water vapor. The reaction therefore becomes autocatalytic and continues until the hydride has been consumed and the entire piece reduced to oxide powder. The amount of nitride required to initiate this reaction is quite small and this nitrogen contamination can occur from a number of sources—hydrogen gas employed, minute leak in the hydriding apparatus or even from degassing of the reaction vessel itself. Longer hydriding times increase the possibility of nitrogen contamination and this is especially true when a dynamic gas system is employed in the hydriding process. The production of stable, solid hydrided yttrium is dependent on the complete absence of nitrogen contamination during processing. If such contamination does occur, powdering of the hydrided product can be prevented by removing the nitride from the surface e.g. grinding or by preventing access of air to the pieces e.g. sealing in wax or plastic. The author wishes to express his appreciation to General Electric Co. for sponsoring this research and for permission to publish the results of work under Subcontract AT-93.

Jan 1, 1962

By Walter Lee Brown

One of the characteristic steps in the march of modern scientific progress is the substitution of improved time-saving and labor-saving appliances for the antiquated and, in most cases, inconvenient forms of chemical and physical apparatus used by the earlier experimenters. This fact is strongly impressed upon us when we consider the question of the employment of illuminating-gas as a source of light, heat and power. Concerning its value as a light-producer, let the record of the past three-quarters of a century speak for itself. As a factor for power, we have evidence of its efficiency in the shape of the gas-engine. But its adaptability as a medium of heat, is the feature to which I wish to call attention, and in a special direction, viz., the assaying of ores. Gas assay-furnaces have been known and used for some years, but not to any very great extent, in this country at least. Therefore no apology on my part is required for the description I now give of a complete gas assaying-plant. The illustration accompanying this paper is a faithful representation of the group, as it was designed by, and arranged for myself, and appears in actual running order in my laboratory to-day. Its duty is to do roasting, crucible-fusion, scorification and cupellation. The furnace at the left is for roasting sulphurets or other ores for experimentation or actual work. It is what is known as a Fletcher No. 163, and consists of a fire-clay body strapped with sheet-iron bands, and a burner (No. 16, Fletcher). The opening at the top

Jan 1, 1885

THE opening session* was held in the hall of the Franklin Institute, on Tuesday evening, June 20th, President Holley in the chair. The President introduced. Mr. Franklin B. Gowen, who addressed the Institute as follows MR. PRESIDENT AND GENTLEMEN : It has been made my pleasant duty to welcome you to the city of Philadelphia, but in so doing I shrink, with some natural reluctance, from appearing before an audience so much better fitted than I am to cope with the subjects which are usually presented to your association, and I can assure you that no trembling neophyte, first venturing within the groves of the Academy, or walking, with sacred reverence, in the gardens of Plato, felt more natural dread at the consequence of his own temerity than I do in appearing before an audience composed of gentlemen belonging to a scientific society of which I am but too sensible that until now I have been a member only in name. In olden times, upon entering a temple sacred to the worship of any deity, it was customary to lay some offering upon the altar, and, in following this custom, it will be my duty, before entering upon the more pleasant part of the task which is assigned me, to call your attention to a subject with which I have been somewhat familiar, and which is entirely within the scope of your investigations, in the belief that I may throw out some hints or some suggestions of a pro¬cess that may be fully developed by some of you, and eventually lead to the introduction of that which may be of service to the human race. The satirist who described the philosopher whom he met, as engaged in the process of extracting sunbeams from cucumbers, * A joint discussion of the subject of Technical Education, by the members of the American Society of Civil Engineers and the American Institute of Mining Engineers, was held in the hall of the Franklin Institute, on Monday evening, June 19th, and Tuesday morning, June 20th. This discussion has been printed in a separate pamphlet by both societies.

Jan 1, 1877