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By W. H. Eardley

IT IS increasingly evident that the excellence of blast-furnace operation to a great extent depends upon the preparation of the products fed into the furnace. The preparation of these products is carried on largely in the roasting and sintering departments. Prior to the building of flotation plants in Utah and other western states for the treatment of lead-zinc ores, the gravity concentrates received at the Midvale smelter amounted to about 4000 tons per month, containing 24 per cent. lead and 10 or 11 per cent. zinc. This product was about 20 mesh-that is, 45 per cent. of it would be plus 20 mesh and the balance minus 20 mesh. About 1000 tons of pyrite per month, containing 5 per cent. lead and 10 per cent. zinc, was also received. These products were sent to the multiple-hearth roasters for calcining, after which they were sent to the Dwight-Lloyd machines for sintering with other ores. The sintering charge passed over the machines but once. The first flotation products received consisted of a wet, sticky, muddy mass, containing a large amount of moisture, up to 19 or 20 per cent., and it was almost impossible to feed .them with any degree of regularity, if at all, through our standard feeders; but the amount of flotation product received during the first year or so was relatively small and it virtually lost its identity by being mixed with a large amount of jig and table concentrates. As the quantity of flotation products increased, more efficient filtering was accomplished and the moisture greatly reduced. FLOTATION PRODUCTS RECEIVED At the present time the Midvale plant receives about 4300 tons per month of flotation product running 60 per cent. lead and 4.5 per cent. zinc, 85 per cent. of which is minus 200 mesh and contains about 8 per cent. moisture; and 4000 tons per month of pyrite of similar fineness, running about 2 per cent. lead and 3.5 per cent. zinc, containing about 10 per cent. moisture. The lower moisture greatly reduces the difficulties of handling, making it possible to run a 100 per cent. flotation feed on a multiple-hearth furnace without serious mechanical troubles. The calcine, however, would contain-nodules and balls of unroasted concentrates, sulfur elimination

Jan 1, 1928

By M. Sagheer

This paper gives a report of the laboratory work investigating the fundamental flotation characteristics of chromite and its commonly associated mineral, serpentine. Floatability curves, showing floatability of chromite at different concentrations of sodium oleate and pH, were obtained by pick-up method. One of the difficulties encountered in flotation of chromite in presence of serpentine has been attributed to dissolved metal ions. The influence of metal ions, dissolved in pulp filtrate, on floatability of pure chromite and serpentine has been studied and it has been shown that Mg, Ca and Fe ions depress chromite. A considerable amount of work applying bubble pick-up method was carried out to counteract the depressing action of metal ions. Various methods and reagents were applied in this connection. Validity of each method and reagent has been discussed. Probably due to the abundance of high-grade chrome ores, very little has been published concerning the flotation of chromite. As improvements in mineral beneficiation are realized, more attention is being directed to low-grade ores previously considered unusable. Currently, gravity concentration is the principal process applied to upgrade chrome ores, but this cannot be used for finely disseminated ore because of the substantial losses in the fines,1,2,3 To avoid these losses, flotation can be applied to material which is too fine for satisfactory gravity concent ration, and it is probable that a combination

Jan 1, 1967

By O. W. Walvoord

A Definition: An ore feeder is a mechanical device that, by virtue of its motion, causes ore to be supplied or carried forward at a desired metered rate to other milling equipment. From the viewpoint of economics there can be little question, even for small tonnage operations, as to the advisability of using mechanical feeders in the place of manual labor. Only a few short years ago, it was common practice to employ crusher men for the feeding of crushers, thus eliminating the capital expenditures required for mechanical feeding equipment. Having been a crusher man in several instances, the author does not favor such practice. The high cost of labor today eliminates the crusher man, and feeders become an economical capital expenditure when considered against the importance of obtaining maximum production efficiency from all the machines in a process flowsheet.

Jan 2, 1955

By F. H. Wilson, E. W. Palmer

The solid solubility of iron in 2 to 10 pct cupro-nickels increases with temperature and nickel content. Property changes accompanying various heat treatments indicate typical precipitation hardening behavior. Iron content also affects softening temperature and sub-scale formation. These factors, as well as impingement corrosion resistance, influence the optimum iron content of commercial alloys. FOR many years Cu-Ni alloys have been used extensively in the form of tubes, pipes, and plates for the construction of salt-water lines and surface condensers on shipboard and in tidewater power stations. The 30 pct Ni alloy has been considered more resistant to rapidly flowing sea water than alloys of lower nickel content, and has been standard on ships of the U. S. Navy. Some ten years ago, the still better corrosion resistance obtained by modifying the 30 pct Ni alloy with approximately 0.5 pct Fe was recognized, and the iron-bearing alloy rapidly superseded the plain alloy as the standard material for severe service. In 1945, Tracy and Hungerford1 published a study of the effect of iron on the corrosion of various cupro-nickels in sea-salt solutions, and their data indicated that the 10 pct Ni alloy containing about 0.75 pct Fe was equivalent to the 30 pct Ni alloy containing 0.5 pct Fe. This was confirmed by LaQue in discussion of the above paper, and by results in an experimental condenser set up at the Kure Beach marine test station of The International Nickel Co., reported by Freeman and Tracy.' The 10 pct Ni iron-bearing alloy is now being very widely used in applications where the 30 pct Ni iron-bearing alloy was formerly considered standard. While this "substitution" has undoubtedly been stimulated by the present extreme shortage of nickel, it must be emphasized that it involves no loss of service performance, and would have occurred anyway in the course of time, for economic reasons. In view of the increasing use of the 10 pct alloy, it seems desirable to make generally available the results of several investigations of Cu-Ni-Fe alloys carried out in the Metallurgical Research Laboratory of The American Brass Co. in recent years. The present paper, deals with the constitution of these alloys in the copper-rich corner of the system, and with the variations in hardness and tensile properties resulting from the heat treatment of alloys containing various amounts of iron. Most of this work is concerned with alloys containing 10 pct Ni. With over about 0.75 pct fe, the 10 pct Ni alloy is suscep- Alloys Several series of cupro-nickel alloys containing iron were used in these investigations. Most of them were prepared in the laboratory, but two samples of commercially fabricated alloys were included. Series A—Nominally 2 and 5 pct Ni, each with 0 to 1.5 pct Fe. Series B—Nominally 10 pct Ni with 0.1 to 0.4 pct Fe. Series C—Nominally 1.0 pct Ni with 0 to 2 pct Fe. Series D—Nominally 10 pct Ni with 3 to 5 pct Fe. Series E—Nominally 10 pct Ni with 1 and 1.5 pct Fe.

Jan 1, 1953

HENRY FAY, Cambridge, Mass. (written discussion *).-Mr. Rawdon has made a distinct contribution to our knowledge of wrought iron, and .perhaps of steel. It will undoubtedly lead to more careful scrutiny of high-phosphorus steels, with perhaps important results. In view of his results, it would seem to be unprofitable to push further any propaganda on the use of higher-phosphorus low-carbon steels until further information is available. As is well known, and as Mr. Rawdon clearly shows, the process of solidification is a selective one, and there is abundant opportunity for those portions of the melt last to solidify to become rich in phosphorus, and the diffusion of this phosphorus-rich area is slow. Hot work does not help the situation appreciably and only serves to concentrate the low-melting material. It is undoubtedly true, as some writers have recently claimed, that the specifications for steels as they. now exist eliminate some perfectly good material. Higher phosphorus in steel may be perfectly safe provided all of the phosphide is completely and uniformly, diffused in the solid solution. If, on the contrary, it is not evenly diffused, and there is a reasonable chance for it not to be, it makes the steel unsafe. Until our knowledge: of the rate of diffusion of phosphorus in steel, and the effect of other elements upon the rate, is more complete, it seems to me unwise, in view of Mr. Rawdon's experiments, to listen to the recommendations for the use of higher-phosphorus steels.

Jan 1, 1918

Jan 1, 1900

By Marc Lemieux

Computer pit design techniques generally make use of models in which the deposit is represented by a regular array of data. Using a regular system, the number of data points required to represent the air, waste and mineralization in a large deposit become excessive. The number of blocks used to describe the deposit is dependent upon the block size. The quality of the pit wall slope design also is dependent upon the block size used and the method of defining the slope. The error associated with reserve calculations becomes greater with increasing block size. A deposit model consisting of variable sized air and mineralized blocks has been developed at the University of British Columbia and improved upon at Climax for pit design work. The method permits put- ting the entire model in core for rapid data processing. This permits the use of a versatile cone generation technique which allows close adherence to variable slope constraints in all directions. The conical shape is approximated by rectangles on each level which equal the area of the ideal conical intersection. The shape of the intersection may vary from approximately circular to elipsoidal. The approximate cone shape is controlled by the slope constraints applicable at the point of intersection on the bench. The overall modeling technique greatly assists the pit design engineer in developing a high quality pit design.

Jan 1, 1977

By P. A. Tucker, C. R. Hudgens, D. E. Etter, D. L. Roesch, D. B. Martin

The equilibrium phase diagram of the Pu-Cd system is presented based on data obtained by differential thermal analysis, metallography, and electron-microprobe X-ray analysis. Liquidus temperatures range from 320° to 934°C. The system contains one congruently melting compound, PuCd, (945°C), and three incongruently melting compounds, PuCd, (800°C), PuCd, (730°C), and PuCd11 (410°C). A liquid-miscibility gap extends from 2 to 60 at. pet Cd with the monotectic reaction isotherm at 910°C. INTEREST in the potential use of plutonium alloys as reactor-fuel materials has prompted investigation of the phase equilibria in plutonium binary systems. A cursory investigation of the phase equilibria in the Pu-Cd binary system was conducted by differential thermal analysis (DTA), metallography, and electron-microprobe X-ray analysis (EMX). Extensive solid solubility of cadmium in both e and 6 plutonium was predicted1 based on atomic radii and electronegativities. Liquid immiscibility between these two elements was also predicted based on Mott's extension of Hildebrand's method. In the only previous investigation of the Pu-Cd system,2 two intermetallic compounds, PuCd11 (incon-gruent melting point 406°C) and PuCd8, were identified. EXPERIMENTAL The plutonium metal used in this work had a total impurity content of 500 ppm; the major impurities were: carbon (215 pprn), silicon (75 ppm), iron (60 ppm), nickel (40 ppm), and aluminum (25 ppm). The cadmium was reagent grade with a purity of 99.99 pet. The DTA technique for the study of plutonium alloys was previously described in detail.3 The alloys to be studied were prepared in tantalum DTA specimen capsules which were sealed by inert-gas welding. The alloys were homogenized in the liquid state in these sealed capsules which prevented the loss of cadmium by vaporization. Only the thermal arrests in the DTA heating curves were used to define the transformation temperatures of the system since supercooling affected many of the results during cooling. After the alloys were analyzed by DTA, the same alloys were used for the metallographic studies. Metallographic examinations were conducted in the manner described for plutonium alloys., No reaction was detected between the alloys and the tantalum capsules. Alloys for EMX analysis were placed in metallographic mounts together with specimens of unalloyed plutonium and cadmium which served as standards. The samples were highly polished but unetched. No protective coatings were applied to the surfaces of these radioactive specimens. Such coatings are detrimental to the excitation conditions and have been found to be unnecessary for the control of radioactive contamination. RESULTS The results of the DTA studies are presented in Table I. The phase diagram, constructed from these data plus the metallographic and EMX results, is presented in Fig. 1. The congruently melting compound, PuCd2, was identified by the occurrence of a maximum melting point (945°C) at 33.3 at. pet Pu-66.7 at. pet Cd and by the presence of a single phase in this composition.

Jan 1, 1965

By C. W. Sherman, J. Chipman, H. I. Elvander

THE pronounced and usually deleterious effects of sulphur on all ferrous metals and the resultant necessity for its control in metallurgical processes have stimulated many investigations of the system iron-sulphur. The data required for thermodynamic study of the behavior of sulphur in molten iron and steel include the activity and free energy of the dissolved sulphur and its heat of solution. Such data are also of theoretical interest since there is all too little information available concerning solutions of nonmetallic solutes in metallic solvents. It was the purpose of this investigation to attack the problem very directly by a study of equilibrium at several temperatures in the reaction H2 (gas) + S = H2S (gas) [1] K1 = PH2S /PH2 as where the sulphur is present in the liquid iron in amounts up to several percent by weight. Such a method of attack is not new since several careful studies have already been reported. It is planned, however, to extend the study to other metallic solvents and particularly to determine the effects of the various alloying elements on the activity of sulphur in liquid iron. This paper presents the results on molten iron-sulphur alloys containing up to 4 pct sulphur in the temperature range 1530°-1730°C. Literature Review The significant researches on dilute molten solutions of sulphur in iron include those of Chipman

Jan 1, 1951

By C. A. Stetefeldt

In my paper on "The Refining of Sulphides Obtained in the Lixiviation-Process with Hyposulphite Solutions," read at Cleveland, June, 1891 (Trans., xx., 37), I recommended the Roessler converter

Jan 1, 1893

By A. B. Young

The difficulties encountered in the preparation of the lead smelter charge for the blast furnace and in the roasting and sintering of the ores, and the expert means taken for the preparation of these materials since the introduction of flotation concentrates into the lead smelter charge, have been described by W. H. Eardleyl and R. A. Wagstaff.² Function of Roasters and Blast Furnaces The lead smelter has first its roasters and its sintering devices, of which the primary object is the removal of sulfur from the ore or from the charge. The blast furnace follows; its function being the elimination of the gangue material left in the charge—the elimination of the insoluble, the iron, the zinc and the lime from the metallic lead. The secondary object is the separation of copper from the lead. A lead blast furnace is a sensitive apparatus. The materials composing the charge must be marshalled in certain proportions before they will make a fluid slag which will separate from the metallic lead. The silica, iron, lime and zinc must be put together in proportions that usually do not mist naturally in the ores, therefore fluxes are necessary. Function of the Flotation Cell The flotation cell—-speaking from the standpoint of a lead concentrate—has taken over part of the work hitherto performed entirely by either gravity concentration or the lead blast furnace. It has eliminated gangue from the concentrate and separated waste products from the lead. In so far as it has done that, it has usurped some of the function of the lead blast furnace; and it is much cheaper to run a flotation cell than a lead blast furnace. The effect in Utah, and it will be similar to effects in other districts. has been to remove a great deal of the gangue by means of flotation, whereas in the old clays it was eliminated by means of sme1ting. In this district, as in others, the insoluble content of the ores has been greatly out of proportion to the iron and lime content to make a proper slag

Jan 1, 1928

By J. W. Downey, M. V. Nevitt

MUELLER and Knott' have reported that Ti2Cu has the Si2Mo-type (Cllb) structure. The lattice parameters of Ti2Cu and the positions of the titanium and copper atoms are given by them as follows: ao = 2.944A; co = 10.786A 6 atoms per unit cell: 2 Cu (a) 000; 1/2: 1/2, 1/2 4 Ti (e) 002; 1/2, 1/2, 1/2 + z 00 -2 ; 1/2. 1/2. 1/2- z where z = 0.341 We have found eight other binary compounds which appear to be isostructural with Ti2Cu. All of them involve the combination of a titanium group element with a copper group element or a titanium group element with palladium. The compounds and their lattice parameters are given in Table I. The alloy samples were prepared by arc melting metals having a purity of 99.9 pct or better. They were homogenized for 72 hr at 900°C in evacuated capsules and quenched in tap water. Filings were prepared, and these were reannealed for 4 hr at 700°C, also in evacuated tubes. The lattice parameters were determined by a least squares Bnalysis of the back reflection lines of patterns made with cobalt radiation. It was not possible to make a precise determination of the lattice parameters of Zr2Au because the filings underwent rapid oxidation at room temperature. The evidence supporting the large tetragonal cell containing 6 atoms involves the presence of the reflections 002, 101, 004, 112, 114, 202, and other reflections with higher indices for which I = 3n. Three or more reflections corresponding to these indices, which cannot be indexed on the basis of a small body-centered tetragonal cell containing 2 atoms, are observed in the patterns of all of the compounds listed in Table I. They are strongest and most numerous when the components have large differences in their atomic scattering factors, as is the case in Ti2Pd, Zr2Cu, and Hf2Cu. The values of the z parameter should be regarded as approximate They were selected on the basis of the best agreement between the observed intensities of two pairs of closely spaced powder pattern lines (004): (112) and (114): (202) and the corresponding intensities calculated for several values of z. An ordering scheme was assumed in which titanium, zirconium, or hafnium atoms occupy the titanium positions of Ti2Cu, and copper, silver, palladium, or gold atoms occupy the copper positions. Calculated and observed intensities of the aforementioned lines and the other lines of the patterns are in satisfactory agreement, but a refinement of the z parameters and a final confirmation of the ordering arrangement must await a more detailed study. It is interesting to note that in transition metal systems at A2B stoichiometry the Si2Mo-type structure competes for stability with two other fre-

Jan 1, 1962

By R. G. Whittemore, R. Derry

Nickel metal, in powder form, has been produced by pressure reduction, with hydrogen gas, of slurries of nickel hydroxide at temperatures up to 250°C. The nickel hydroxide was obtained by precipitation from nickel chloride and nickel sulphate solutions, using both magnesium oxide and calcium oxide. Rates of reduction and yields were determined as a function of temperature, hydrogen overpressure, seed addition, and the amount of alkali used. The mechanism of reduction of slurries obtained from the sulphate system was studied, and major differences between the sulphate system and the previously examined chloride system investigated. Specifically, in the sulphate system, contra the chloride system, no seeding was necessary, plating and densification were virtually absent and only short induction periods occurred. Grades of product are given and the use of this process in the recovery of nickel from laterites is discussed. The selective reduction of nickel from mixed hydroxide slurries and effluent treatment plant sludge has also been examined.

Jan 1, 1973

By H. K. Birnbaum, H. B. Aaron

he authors suggest that a number of the types of yield phenomena which have been observed in high-purity fcc metals are due to dislocation interactions bccurring at the surface of the crystals rather than due to volume effects. Since rather different inter-pretationS2,7,12,14,15,21-23 of these effects have been suggested, it is of some importance to ascertain the role of the surface in these yield phenomena. It should be first noted that the high-purity fcc metals appear to exhibit several distinct types of yield phenomena. The "unloading yield point" which is observed on reloading the specimen after removing the applied load has been found to be independent of the time of holding in the unloaded condition. If however the specimen is aged while under load and re-tested without removing the load, a yield point is observed which does depend on the aging time and tem-perature. Feng and Kramer suggest that the removal of the unloading yield point on removing sufficient material from the surface of the specimen indicates that the effect is associated with dislocation interactions at the specimen surface. Their observations are counter to those of Haasen and Kelly5 and Birnbaum.12 Since the unloading yield points are extremely small (-2 pct of the flow stress) the results of the surface removal will depend on whether the material is removed uniformly over the gage length. The introduction of small etch pits or the removal of more material from one portion of the specimen than from another will result in preferential yielding and obliteration of the yield point. With the normal electropolishing techniques it would be difficult to avoid these effects. The data obtained by Aaron and Birnbaum, Fig. 10, on aluminum polycrystalline specimens indicate that, although the unloading yield point and the strain-aging yield point are not simply additive, a time- and temperature-dependent yield point is observed under conditions where no creep is observed. This does not agree with the results of Feng and Kramer but does agree with the results on copper15 and gold.7~23 The source of the discrepancy may be the procedure used by Feng and Kramer to correct their time-dependent yield points for the effect of creep. Since the strain-aging yield point is not independent of the pre-aging strain rate, Fig. 11, the effects of creep cannot

Jan 1, 1967

Jan 1, 1951

Jan 1, 1951

By George Breyer

DURING the past 25 years the steelmaker has experienced some difficulty in producing steel to meet the standards established by the metallurgist. In contrast to the past, when a chemical specification of broad limits was the only requirement, he now has to employ such tests as microscopic, macroscopic, tensile, impact, Magnaflux and even X-ray and supersonic. The development of these tests has more than set the pace for a manufacturing process of which the exactness still hinges to an important degree on the ability of the furnace operator. In our efforts to produce steel, and especially alloy steel, to meet the exactness of modern engineering specification, many factors must be taken into account. It is not sufficient to make a good heat of steel in the furnace and then be satisfied that the job is done, since there are many pitfalls between the furnace and the finished product. The literature abounds with information on melting practices, deoxidation methods and slag control, but the lack of positive information about what happens when the steel is teemed into molds is quite evident. Such questions as what is the proper mold size, shape and thickness; which is the best mold coating; what is the best rate of pour for any given steel, and what is the effect of cooling rates on quality, are still answered by opinions. It is acknowledged that a poor heat of steel cannot be improved in the pouring pit. On the other hand, a good heat can be ruined by improper handling after it leaves the furnace.

Jan 1, 1947

By F. M. Lewis, J.F. Myers

The Tennessee Copper Company's operations are in the Ducktown Basin, in the extreme southeast corner of Tennessee. The ore is of the heavy sulphide type, the predominating sulphides being pyrite, pyr-rhotite, chalcopyrite and sphalerite. The gangue is a micaceous schist, with varying amounts of free quartz. The mining operation develops two classes of ore, each of which is concentrated by the flotation process in separate mills. Table 1 shows a typical analysis of the ore treated in each mill. The London mill was built in 1922, with a capacity of 400 tons per day. This was gradually increased to 600 tons by 1926, to 900 tons in 1928, and to 1350 tons in 1938. Fig. 1 shows the crushing and grinding flowsheet in 1928, when the capacity was 900 tons; Fig. 2, the crushing and grinding flowsheet that was developed by 1938, for the treatment of 1350 tons per day. A comparison of these flowsheets reveals that this increase in tonnage, with a subsequent improved operation, was accomplished with identically the same major equipment. Improving a concentrator's capacity, metallurgical results, and costs as time goes by is a commonplace practice, and is accomplished in various ways, depending upon the local conditions. The reason for presenting the data of how this was accomplished in the mills of the Tennessee Copper Co. is that a fast-running rod mill plays such an interesting role

Jan 1, 1943

By J. F. Myers, F. M. Lewis

The Tennessee Copper Company's operations are in the Ducktown Basin, in the extreme southeast corner of Tennessee. The ore is of the heavy sulphide type, the predominating sulphides being pyrite, pyr-rhotite, chalcopyrite and sphalerite. The gangue is a micaceous schist, with varying amounts of free quartz. The mining operation develops two classes of ore, each of which is concentrated by the flotation process in separate mills. Table 1 shows a typical analysis of the ore treated in each mill. The London mill was built in 1922, with a capacity of 400 tons per day. This was gradually increased to 600 tons by 1926, to 900 tons in 1928, and to 1350 tons in 1938. Fig. 1 shows the crushing and grinding flowsheet in 1928, when the capacity was 900 tons; Fig. 2, the crushing and grinding flowsheet that was developed by 1938, for the treatment of 1350 tons per day. A comparison of these flowsheets reveals that this increase in tonnage, with a subsequent improved operation, was accomplished with identically the same major equipment. Improving a concentrator's capacity, metallurgical results, and costs as time goes by is a commonplace practice, and is accomplished in various ways, depending upon the local conditions. The reason for presenting the data of how this was accomplished in the mills of the Tennessee Copper Co. is that a fast-running rod mill plays such an interesting role

Jan 1, 1943

By S. C. Sircar, D. R. Wiles

The rate has been studied of the hydrogen reduction of nickel ions in acetate -buffered solutions, using a nickel catalyst. At temperatures between 130°and 160°C, the rate is found to be proportional to the catalyst area, the nickel ion concentration, and the hydrogen pressure. The effect of hydrogen ions is to reduce the observed rate, likely by causing the reverse reaction (dissolution) to proceed. The experimental activation energy was found to be 25 kcal per mole. THE precipitation of metals and lower oxides from solution by hydrogen reduction has been quite actively investigated during the past few years.1 In the case of nickel, the kinetics of the precipitation have been studied in ammonia solution2 but extension of this study to acid solutions has not attracted much interest, largely because of the unfavorable thermodynamics at all but the lowest acidities. For example, Schaufelberger foundg that only 10 pct reduction of nickel could be effected in sulphate solutions. One kinetic study of the reduction of Ni++ has been reported by Knacke, Pawlek, and Sussmuth,4 in which the order of the reaction was found to be one in nickel ion and one-half in hydrogen pressure. No mention was made as to the part played by the nickel catalyst, or by the pH of the solution. Moreover, the activation energy reported (4 .12 kcal per mole) is so low as to lead to some question as to whether diffusion might be playing a major role in determining the kinetics. We have recently completed a study5 of the kinetics of the hydrogen precipitation of nickel from acetate-buffered acidic solutions whose results confirm and amplify those of Knacke et al. EXPERIMENTAL PROCEDURES The work was done in a high-pressure autoclavee by the usual technique of removing small samples of the solution for analysis. Nickel analysis was done colorimetrically by the dimethylglyoxime method.' The catalyst used was carbonyl nickel powder (Standard A powder of the Mond Nickel Co., Ltd.) which was found to be composed of spheres of less than 350 mesh. The surface area of the powder was determined in this laboratory by the B. E. T. method to be 1.85 sq m (m2) per g. The catalyst was added to the solution only after the proper temperature and pressure had been reached. Agitation of the baffled system was by a turbine-type impeller, rotated at speeds between 400 and 750 rpm. The reduction rate was found to be independent of the stirring rate, so it was assumed that diffusion in the liquid does not limit the rate. In typical experiments, the nickel concentration was unchanged during an induction period of variable length. The concentration then decreased sharply, and gradually levelled off to approach the final equilibrium value. In some cases, notably at high stirring rates, the nickel concentration was found to increase considerably during the induction period, and then to decrease. In all cases, the rate was determined from the slope of the tangent to the rate curve as the concentration first decreased below the initial value. This is seen in Fig. 1. The rate measurements were found to be reproducible to within about 5 and to be quite independent of the nature or duration of the induction period. The range of conditions used is given in Table I.

Jan 1, 1961