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By A. A. Jr. Smith, J. S. Smart

Numerous investigations of the effects of the various impurities common to commercial coppers have been published, and the data have found wide use in industry. Naturally, emphasis has been placed on the oxygen-bearing coppers of the tough-pitch variety, but need is now evident for data covering the oxygen-free condition as well. Furthermore, relatively few of the important reactions between oxygen and the various impurities are well understood, and often the data at hand are not applicable to the low concentrations encountered in commercial coppers. This paper presents the changes in conductivity and softening temperature derived from individual additions of the group VIII triad, iron, cobalt and nickel, to high-purity copper, and constitutes a portion of the copper-research program being conducted at the Central Research Laboratory of the American Smelting and Refining Co. The method of preparation of high-purity copper and its alloys in either the oxygen-free or oxygen-bearing form has been described previous1y.l The purity of this material, and the methods developed to produce it, provide the means for direct investigation of the very low concentration range in which the various impurities generally exist in commercial coppers. The usual necessity for extrapolation to this range using the results obtained from higher concentrations, and the interfering effects of extraneous impurities, are thus simultaneously circumvented. Since previously published data have adequately presented the effects of higher concentrations of iron, cobalt and nickel, the present investigation has been confined to the composition range o to 0.05 per cent. All alloys were initially prepared in the form of oxygen-free continuous cast rod, the weighed alloying additions in suitable form being charged with the pure copper to the continuous casting crucible. The best of the available high-purity alloying materials were used, and spectrographic analyses confirmed the absence of interfering elements from the alloys formed. Each series was compounded in the direction of increasing concentration, starting with pure copper in a new crucible and finishing with the 0.05 per cent alloy. Composition was closely controlled by adding the alloying element in the form of a carefully compounded and analyzed master alloy rendered uniform by continuous casting. The accuracy of this method of synihesis was proved by chemical analysis of the more concentrated alloys, and, accordingly, there is every reason to credit the stated composition of the very dilute alloys in the range where chemical analysis becomes highly uncertain. Oxygen-free samples for measurements of conductivity and softening temperature Were obtained by drawing the continuous cast rod to wire of 0.08I-in. diameter. employing a number of intermediate anneals to refine the grain structure. The

Jan 1, 1942

By A. A. Jr. Smith, J. S. Smart

Numerous investigations of the effects of the various impurities common to commercial coppers have been published, and the data have found wide use in industry. Naturally, emphasis has been placed on the oxygen-bearing coppers of the tough-pitch variety, but need is now evident for data covering the oxygen-free condition as well. Furthermore, relatively few of the important reactions between oxygen and the various impurities are well understood, and often the data at hand are not applicable to the low concentrations encountered in commercial coppers. This paper presents the changes in conductivity and softening temperature derived from individual additions of the group VIII triad, iron, cobalt and nickel, to high-purity copper, and constitutes a portion of the copper-research program being conducted at the Central Research Laboratory of the American Smelting and Refining Co. The method of preparation of high-purity copper and its alloys in either the oxygen-free or oxygen-bearing form has been described previous1y.l The purity of this material, and the methods developed to produce it, provide the means for direct investigation of the very low concentration range in which the various impurities generally exist in commercial coppers. The usual necessity for extrapolation to this range using the results obtained from higher concentrations, and the interfering effects of extraneous impurities, are thus simultaneously circumvented. Since previously published data have adequately presented the effects of higher concentrations of iron, cobalt and nickel, the present investigation has been confined to the composition range o to 0.05 per cent. All alloys were initially prepared in the form of oxygen-free continuous cast rod, the weighed alloying additions in suitable form being charged with the pure copper to the continuous casting crucible. The best of the available high-purity alloying materials were used, and spectrographic analyses confirmed the absence of interfering elements from the alloys formed. Each series was compounded in the direction of increasing concentration, starting with pure copper in a new crucible and finishing with the 0.05 per cent alloy. Composition was closely controlled by adding the alloying element in the form of a carefully compounded and analyzed master alloy rendered uniform by continuous casting. The accuracy of this method of synihesis was proved by chemical analysis of the more concentrated alloys, and, accordingly, there is every reason to credit the stated composition of the very dilute alloys in the range where chemical analysis becomes highly uncertain. Oxygen-free samples for measurements of conductivity and softening temperature Were obtained by drawing the continuous cast rod to wire of 0.08I-in. diameter. employing a number of intermediate anneals to refine the grain structure. The

Jan 1, 1942

By Paul A. Beck

It is well known that the hardness of metallic single crystals, like that of polycrystalline metals, increases during deformation (hardening by cold-work). It is also known that, as a consequence of deformation. the metallic material acquires an evident thermodynamic instability, revealed, for example, by the fact that the increased hardness gradually decreases with time, especially at elevated temperatures (softening by annealing). The temperature at which the stabilizing process begins is different for various metals, and for any metal it depends on the amount of deformation. Such stabilization of deformed metals may proceed in two different ways: through recovery, and through recrystallization. The former process allows the unstable deformed metal body to approach stability gradually and without visible change in the grain structure; the latter process, like an allotropic transformation, yields directly the undeformed stable "phase" in the form of new undeformed crystals, which, starting out of a certain number of nuclei, grow into and " consume " the deformed hard material. The extent of stability attainable through recovery is limited, especially if the deformation of the metal crystal or crystals involves not only the gliding along slip planes, but also the bending of the slip lamellae, or at any rate the bending of comparatively large parts of the crystal lattice. In such cases, for instance in bent single crystals or polycrystalline metals subjected to any deformation, recovery will not as a rule be able to restore the "istraight" undeformed lattice, and stability can be attained only by recrystallization; that is, by the consumption of the bent crystal lattice parts by new, undeformed crystals—a much more drastic process. It is evident that the part of the surplus free energy stored in deformed crystals, which is present in the form of the elastic energy of the bent lamellae, is in these instances not considerably involved

Jan 1, 1937

By Herbert H. Kellogg

Deposits of high-silica kaolinite clays occur at many places in central Pennsylvania. These white clays were formed apparently by weathering of argillaceous quartzite and limestone. Their geology, distribution and use have been reported by Leighton.1 The larger deposits have been mined from time to time, and the clay, after washing to remove coarse sand, has found use as rubber filler, foundry clay, and in white cements. In general, the clay from these deposits contains too much grit (quartz) to be useful as paper filler, and the silica content is too high to make it useful as china clay for ceramic ware. Gravity methods for the separation of quartz from these clays have failed because of the extremely fine size of the quartz grains, but by the methods of froth flotation described in this paper these sandy kaolins can be made to yield a purified kaolinite that has a chemical composition close to that of good-grade Georgia kaolins, and is free enough from grit to be used as a paper filler. As by-products of the separation, a fine (— 325-mesh) sand assaying 95.5 per cent SiO2, and a very he (—3-micron) clay are produced. The possible ceramic uses of these products are being investigated at The Pennsylvania State College. Experimental Procedure The Sample.—The clay sample used in these tests was obtained from a small mine near Tyrone, Pa. It had already been washed to remove coarse sand, and represented the finished product of this small mine and washery. Microscopic examination showed that the clay was composed almost entirely of the minerals quartz and kaolinite, and that the quartz was present mostly in particles larger than one micron, while the kaolinite particles generally were less than 20 microns in size. The kaolinite and quartz particles were physically separable by blunging the clay in water with a suitable dispersant. Preparation of Flotation Feed.—By the addition of NaOH in an amount equal to 3 lb. per ton of solids, the clay was completely dispersed in water. Flotation feed was prepared by allowing a dispersed suspension (10 per cent solids) of the clay to stand for the period of time required for a 2.5-micron particle of quartz to settle from the top of the container to the bottom. After this settling period the suspension was decanted from the settled solids. The settled solids were redispersed in water and the separation was repeated once. The two fine fractions were then combined. Thus the clay was divided into a fine and a coarse fraction by size separation at approximately 2.5 microns.* The fine fractioh was found to have a considerably lower sand content than the raw clay (Table I), and was not treated further. The coarse fraction formed the flotation feed for all the tests described in this paper. A size separation of this type can be

Jan 1, 1947

By Herbert H. Kellogg

Deposits of high-silica kaolinite clays occur at many places in central Pennsylvania. These white clays were formed apparently by weathering of argillaceous quartzite and limestone. Their geology, distribution and use have been reported by Leighton.1 The larger deposits have been mined from time to time, and the clay, after washing to remove coarse sand, has found use as rubber filler, foundry clay, and in white cements. In general, the clay from these deposits contains too much grit (quartz) to be useful as paper filler, and the silica content is too high to make it useful as china clay for ceramic ware. Gravity methods for the separation of quartz from these clays have failed because of the extremely fine size of the quartz grains, but by the methods of froth flotation described in this paper these sandy kaolins can be made to yield a purified kaolinite that has a chemical composition close to that of good-grade Georgia kaolins, and is free enough from grit to be used as a paper filler. As by-products of the separation, a fine (— 325-mesh) sand assaying 95.5 per cent SiO2, and a very he (—3-micron) clay are produced. The possible ceramic uses of these products are being investigated at The Pennsylvania State College. Experimental Procedure The Sample.—The clay sample used in these tests was obtained from a small mine near Tyrone, Pa. It had already been washed to remove coarse sand, and represented the finished product of this small mine and washery. Microscopic examination showed that the clay was composed almost entirely of the minerals quartz and kaolinite, and that the quartz was present mostly in particles larger than one micron, while the kaolinite particles generally were less than 20 microns in size. The kaolinite and quartz particles were physically separable by blunging the clay in water with a suitable dispersant. Preparation of Flotation Feed.—By the addition of NaOH in an amount equal to 3 lb. per ton of solids, the clay was completely dispersed in water. Flotation feed was prepared by allowing a dispersed suspension (10 per cent solids) of the clay to stand for the period of time required for a 2.5-micron particle of quartz to settle from the top of the container to the bottom. After this settling period the suspension was decanted from the settled solids. The settled solids were redispersed in water and the separation was repeated once. The two fine fractions were then combined. Thus the clay was divided into a fine and a coarse fraction by size separation at approximately 2.5 microns.* The fine fractioh was found to have a considerably lower sand content than the raw clay (Table I), and was not treated further. The coarse fraction formed the flotation feed for all the tests described in this paper. A size separation of this type can be

Jan 1, 1947

By O. C. Ralston

Flotation is now commonly practiced in alkaline ore pulps, yet little is known regarding the action of the alkaline solutions on the ore particles beyond the fact that films of oxidized material form. We wish to chronicle our discovery of the presence of soluble reducing agents in alkaline ore pulps of the United Verde, and present some data on lime consumption. During the grinding and flotation of a pyritic ore containing small amounts of ferrous sulfate and other soluble salts, an excess of lime was added to precipitate the salts, and filtered samples of the solution were titrated with standard permanganate solution. Even in pulps of high causticity an appreciable permanganate titration was always obtained, in spite of the fact that the solutions were shown to contain little iron. Investigation of the cause brought about the discovery of several previously unsuspected compounds in flotation pulps made from pyritic ore. Not only the reducing agents present had to be identified, but also the amount of dissolved oxygen, and a survey was finally made of the free oxygen content and reducing agents of the mill pulp in the concentrating mill at Clarkdale. A great many compounds might form, caused by oxidation of pyrite or other metal sulfides or by reaction between a lime solution and pyrite. The most probable compounds considered were calcium sulfides, polysul-fides, thiosulfates, and polythionates. Later it was discovered in the literature that in alkaline pulp polythionates do not exist and if introduced are decomposed into sulfites and thiosu1fates.l Any precipitated sulfur is changed by alkali into thiosulfate and polysulfide. Sulfites and sulfides react to form thiosulfate, so that in the end it is possible to have in an alkaline solution only thiosulfate and an excess either of sulfide or sulfite. Confirmatory tests were made and it was finally established that the alkaline mill pulps made from the United Verde ore contained

Jan 1, 1930

By A. W. Fahrenwald

Cell depth has been for many years a controversial question in a flotation-machine performance. In the impeller type of machine, we are really talking about impeller submergence—i.e., the depth in the pulp at which the impeller is required to produce aeration. The Flotation Machine a Compressor A flotation machine can be considered as an air compressor or blower in which the aeration mechanism takes in air under atmospheric pressure† (14.7 Ib. per sq. in.) and blows it into the pulp (the pulp being the receiver) against a head of 14.7 plus cell depth in feet times 0.4333 lb. per sq. inch. In commercial machines the impeller is submerged in the pulp to depths ranging from about 2 ft. in the smaller machines to as much as 5 ft. in some of the larger ones. In the 2-ft. cell, the hydrostatic head on the impeller is (2 X 1.25 =) 2.50 ft. (assuming a pulp density of 1.25), equal to (2.50 X 0.4333 =) 1.078 Ib. per sq. in. For the 5-ft. cell, the hydrostatic head against which the impeller must make air is (5 X 1.25 X 0.4333 =) 2.708 Ib. per sq. inch. In the small 2-ft. machine, the volume reduction is (1.078 ÷ 0.147 + 0.01078 =) 6.85 per cent and in the large, 5-ft. machine, the volume reduction is (2.708 0.147 + 0.02708 =) 15.5 per cent. It is obvious that for unit volume of free air intake the larger machine receives a lesser (8.65 per cent less) volume of aeration* than the smaller machine. The bubbles in escaping from the pulp expand and are greater in volume at the surface than at the moment of their formation in the pulp; 7.33 and 18.4 per cent larger, respectively, in the small and large machines. Just how this situation affects flotation is not known. It is interesting to note, however, that the bubbles are smaller in the zone of the coarsest particles and largest in the upper zones of the her, more easily suspended mineral particles. It would seem that the relationship might be reversed advantageously. The deep cell is at a greater disadvantage in this respect than the shallow cell. Nothing, however, presumably can be done about this situation. The shallow cell is a partial corrective. Not only does the compression ratio of aeration increase with impeller submergence but the hydrostatic head against which the impeller must operate also increases. The Flotation Machine as a Pump Since, in impeller machines that rely upon their own operation to produce aeration, pulp Passes through the im-

Jan 1, 1947

By A. W. Fahrenwald

Cell depth has been for many years a controversial question in a flotation-machine performance. In the impeller type of machine, we are really talking about impeller submergence—i.e., the depth in the pulp at which the impeller is required to produce aeration. The Flotation Machine a Compressor A flotation machine can be considered as an air compressor or blower in which the aeration mechanism takes in air under atmospheric pressure† (14.7 Ib. per sq. in.) and blows it into the pulp (the pulp being the receiver) against a head of 14.7 plus cell depth in feet times 0.4333 lb. per sq. inch. In commercial machines the impeller is submerged in the pulp to depths ranging from about 2 ft. in the smaller machines to as much as 5 ft. in some of the larger ones. In the 2-ft. cell, the hydrostatic head on the impeller is (2 X 1.25 =) 2.50 ft. (assuming a pulp density of 1.25), equal to (2.50 X 0.4333 =) 1.078 Ib. per sq. in. For the 5-ft. cell, the hydrostatic head against which the impeller must make air is (5 X 1.25 X 0.4333 =) 2.708 Ib. per sq. inch. In the small 2-ft. machine, the volume reduction is (1.078 ÷ 0.147 + 0.01078 =) 6.85 per cent and in the large, 5-ft. machine, the volume reduction is (2.708 0.147 + 0.02708 =) 15.5 per cent. It is obvious that for unit volume of free air intake the larger machine receives a lesser (8.65 per cent less) volume of aeration* than the smaller machine. The bubbles in escaping from the pulp expand and are greater in volume at the surface than at the moment of their formation in the pulp; 7.33 and 18.4 per cent larger, respectively, in the small and large machines. Just how this situation affects flotation is not known. It is interesting to note, however, that the bubbles are smaller in the zone of the coarsest particles and largest in the upper zones of the her, more easily suspended mineral particles. It would seem that the relationship might be reversed advantageously. The deep cell is at a greater disadvantage in this respect than the shallow cell. Nothing, however, presumably can be done about this situation. The shallow cell is a partial corrective. Not only does the compression ratio of aeration increase with impeller submergence but the hydrostatic head against which the impeller must operate also increases. The Flotation Machine as a Pump Since, in impeller machines that rely upon their own operation to produce aeration, pulp Passes through the im-

Jan 1, 1947

By John Mark Patek

Knowledge of the relative floatability of silicate minerals is increasing in importance as flotation is being applied to the concentration of nonsulfides. Many silicates are in themselves commercial products amenable to concentration by flotation. Moreover, the selective flotation of other nonsulfide minerals, such as cassiterite, depends largely upon the floatability of associated gangue silicates. Differences in floatability existing between the various silicates have not- been sufficiently appreciated; for example, the feldspars that differ greatly in floatability have generally been merely treated as "feldspar." It was the purpose of the work described in this paper to determine by experiment the differences in floatability between silicates; to investigate the causes for such differences, and to discover a means of predetermining approximate floatability without the necessity of experimentation. Determining Floatability The relative floatability of 20 silicates so selected as to represent all of the more common silicate types1 was obtained by flotation tests enumerated in Table 1. The mineral to be floated was crushed dry on a steel plate, and screened repeatedly during crushing through an 80-mesh screen in order to produce a sand with all grains as close to 80 mesh as possible. The sand was placed in dilute (6N) hydrochloric acid until free of soluble foreign material, and then washed with tap water about ten times in order to remove both acid and fines. The resultant product, which averaged 82 per cent plus 200 mesh, was floated in 50-gram charges in a 50-gram Denver celluloid flotation machine with 0.008 gram of terpineol, and from 0.01 to 0.05 gram of oleic acid in a solution acidified with sulfuric acid. The degree of separation of one mineral from another was determined by counting under a nlicroscope the grains of each mineral, both in the concentrate and in the tailings, and comparing their relative abundance in each. Unless the comparison showed a decided difference in amount,

Jan 1, 1935

By A. B. Cox, L. W. Wark

In an earlier paper1 measurements of contact angles due to the effect of xanthates on mineral surfaces were reported. The solutions in which these measurements were made differed widely from those of modern flotation circuits. It is intended, however, by introducing, one at a time, the other principal reagents of flotation, to approach gradually the solution composition of flotation liquors. The work now described is an attempt to determine the effect of one of the most important of these reagents—namely, sodium cyanide—on the establishment of air-mineral contact. The work has been carried out for the following companies: Broken Hill South, North Broken Hill, Zinc Corporation, Electrolytic Zinc of Australasia, Mount Lyell Mining and Railway, and Burma Corporation. Since the effect of cyanide is inseparably connected with the alkalinity, the results cited below deal with the mutual effects of alkalis and cyanide. Alkalis alone exert a significant effect on the air-mineral contact but comparatively large amounts are required. Since the addition of a small amount of cyanide greatly decreases the degree of alkalinity necessary for the suppression of contact at surfaces of any of the minerals experimented with (except galena) and since alkalis are rarely used alone in practice, little attention has been paid to cyanide-free solutions. It was shown in the previous paper that, excluding the dixanthogen effect, whenever contact was practicable at all in an ethyl xanthate solution the angle of contact was 60". There is, therefore, less necessity to measure equilibrium contact angles; in fact, the experiments herein described have generally been conducted with a view to determining whether contact is possible and not to measuring the actual value of the contact angle. The separations which have generally to be effected in dealing with complex sulfide ores are: (1) galena from sphalerite, pyrite, etc.; (2) sphalerite from pyrite and/or gangue minerals; (3) copper minerals from pyrite and gangue minerals; (4) pyrite from gangue minerals; (5) chal-

Jan 1, 1935

By Harry Seltz, J. C. DeHaven

InteRmetallic compounds are formed in many binary metal systems. Some compounds are stable to their melting points, and others decompose at lower transition temperatures. Even those of the first class are dissociated in the liquid state, as indicated by the continuous form of their solubility curves at their melting points1. While the lattice structures of some of these compounds have been determined, their thermodynamic properties have not been investigated. In this paper is described the determination of the free energy and heat of formation of the compound CdSb, which is of the first class mentioned above, melting congruently at 455' C. This compound shows a rhombic structure, and the lengths of the edges of the elementary cell containing four molecules are: a = 6.52, b = 8.60, c = 4.16 A.' There are three possible methods of determining the free energy of formation of a compound of this type. The first method, applying the third law of thermodynamics, requires the measurement of its heat capacity preferably to liquid hydrogen temperatures, and a calorimetric determination of its heat of formation. The second method involves the study of the equilibrium of the compound in some gas reaction, such as: CdSb + CO² = CdO + CO + Sb From the known free energies of formation of CdO, CO² and CO the free energy of formation of CdSb could be calculated. The third method measures the electromotive force of a galvanic cell in which the cell reaction is the reversible formation of the compound from the elements. The first method is generally applicable, but requires elaborate experimental equipment. The second method can not be used for compounds melting at low temperatures, owing to the difficulty in establishing equilibrium. The electromotive force method, therefore, seemed to offer

Jan 1, 1935

By J. C. DeHaven, Harry Seltz

InteRmetallic compounds are formed in many binary metal systems. Some compounds are stable to their melting points, and others decompose at lower transition temperatures. Even those of the first class are dissociated in the liquid state, as indicated by the continuous form of their solubility curves at their melting points1. While the lattice structures of some of these compounds have been determined, their thermodynamic properties have not been investigated. In this paper is described the determination of the free energy and heat of formation of the compound CdSb, which is of the first class mentioned above, melting congruently at 455' C. This compound shows a rhombic structure, and the lengths of the edges of the elementary cell containing four molecules are: a = 6.52, b = 8.60, c = 4.16 A.' There are three possible methods of determining the free energy of formation of a compound of this type. The first method, applying the third law of thermodynamics, requires the measurement of its heat capacity preferably to liquid hydrogen temperatures, and a calorimetric determination of its heat of formation. The second method involves the study of the equilibrium of the compound in some gas reaction, such as: CdSb + CO² = CdO + CO + Sb From the known free energies of formation of CdO, CO² and CO the free energy of formation of CdSb could be calculated. The third method measures the electromotive force of a galvanic cell in which the cell reaction is the reversible formation of the compound from the elements. The first method is generally applicable, but requires elaborate experimental equipment. The second method can not be used for compounds melting at low temperatures, owing to the difficulty in establishing equilibrium. The electromotive force method, therefore, seemed to offer

Jan 1, 1935

By C. A. Edwards

Following a brief introduction, an outline is given of the four main conditions in which gases may be associated with metals; namely, (1) adsorbed gases, (2) dissolved gases, (3) gases in chemical combination, (4) gases entrapped in blowholes or cavities. Adsorption is essentially a surface phenomenon and is regarded as the attachment of outside molecules or atoms to the exposed free valencies of the atoms comprising the surface layers. In many cases where adsorbed films of gas are formed this is accompanied by a process of diffusion of the gas into the metal itself. This is particularly true in respect to iron and hydrogen, and experiments have shown that there is no difference between the rate at which hydrogen diffuses through a single crystal of iron arid through the same material after it has been recrystal-lized into a mass of small crystals. This does not prevent a somewhat greater concentration of gas at the boundaries of adjacent crystals, nor does it mean that the effect of the gas will be the same at the boundaries as it is within the body of the crystals. Indeed, under certain conditions, iron is rendered very brittle at the crystal boundaries, as shown in experiments by Pfeil with samples of almost pure iron. Much work has been done by many investigators concerning the temperature and conditions under which dissolved hydrogen, in particular, can be at least partially removed from different metals. With iron, the hydrogen that has diffused into the metal as a result of acid attack by pickling or by electrolytic deposition of the gas on the metal is partly removed by exposing the metal to the atmosphere at ordinary temperatures. Considerably more can be eliminated by raising the temperature, and even greater quantities by jointly raising the temperature and reducing the pressure. Annealing at suitable temperatures completely removes the bad effects of excessive mounts of hydrogen dissolved in or associated with iron. This is shown by the data plotted in Fig. 1, giving values for electrolytic iron sheets after annealing at temperatures between 250" and 950" C. The hydrogen brittleness is rapidly diminished at

Jan 1, 1935

By C. A. Edwards

Following a brief introduction, an outline is given of the four main conditions in which gases may be associated with metals; namely, (1) adsorbed gases, (2) dissolved gases, (3) gases in chemical combination, (4) gases entrapped in blowholes or cavities. Adsorption is essentially a surface phenomenon and is regarded as the attachment of outside molecules or atoms to the exposed free valencies of the atoms comprising the surface layers. In many cases where adsorbed films of gas are formed this is accompanied by a process of diffusion of the gas into the metal itself. This is particularly true in respect to iron and hydrogen, and experiments have shown that there is no difference between the rate at which hydrogen diffuses through a single crystal of iron arid through the same material after it has been recrystal-lized into a mass of small crystals. This does not prevent a somewhat greater concentration of gas at the boundaries of adjacent crystals, nor does it mean that the effect of the gas will be the same at the boundaries as it is within the body of the crystals. Indeed, under certain conditions, iron is rendered very brittle at the crystal boundaries, as shown in experiments by Pfeil with samples of almost pure iron. Much work has been done by many investigators concerning the temperature and conditions under which dissolved hydrogen, in particular, can be at least partially removed from different metals. With iron, the hydrogen that has diffused into the metal as a result of acid attack by pickling or by electrolytic deposition of the gas on the metal is partly removed by exposing the metal to the atmosphere at ordinary temperatures. Considerably more can be eliminated by raising the temperature, and even greater quantities by jointly raising the temperature and reducing the pressure. Annealing at suitable temperatures completely removes the bad effects of excessive mounts of hydrogen dissolved in or associated with iron. This is shown by the data plotted in Fig. 1, giving values for electrolytic iron sheets after annealing at temperatures between 250" and 950" C. The hydrogen brittleness is rapidly diminished at

Jan 1, 1935

By Donald F. Irwin

Amid the violent economic changes of recent years that have affected Canadian gold-mining operations so deeply, the discovery and early developments of Kirkland Lake might easily be overlooked. There was more than one "false dawn" for the district before developments finally established the fact of a superb mineralized zone extending through the present operating properties. Never far from the railway, Kirkland Lake has had the benefit of direct rail service for many years. The pioneer discovery on which the first mill and cyanide plant was erected was the "Tough-Oakes," this property being on what is now the eastern end of the producing area; some time later, the "Lake Shore" was discovered at the present center of the district, and a small plant was built upon it also. Both of these early treatment plants were of pre-war design. Progress in gold metallurgy has caused a gradual change in cyanide practice since the early days at Kirkland Lake, which may be observed in the various plants now operating there. From the beginning, it was recognized that Kirkland Lake ores were more responsive to cyanidation than to alternative recovery methods, and that their mineralization contained gold in very finely divided form. Although sulfides and tellurides are present, the quantity is small, being in the order of 1 or 2 per cent by weight, so that gravity concentration is undesirable, since gold is not confined to the sulfides. Some complication is offered by the presence of tellurides, which have caused lengthy controversy over their importance in recovery methods, but which are now generally regarded as less harmful in the light of increasingly high recoveries being obtained. Nevertheless, finely divided gold intimately associated with sulfides in the presence of tellurides; and occurring in the hard Kirkland Lake porphyry ore, substantially free from natural slime-forming constituents, indicates fine grinding. This has been the universal practice although the degree of grinding has varied a little among the different mills and is considerably finer now than formerly. The natural condition as outlined caused the establishment of fine grinding at an early stage in the development of Kirkland Lake, during the period of valuation of gold at, $20.67 per ounce. With the arrival

Jan 1, 1935

By Norman Hedley, George Barsky, S. J. Sawinson

The cyanidation of precious-metal ores is a complex chemical process. Numerous reactions occur, some of which cause an undesired consumption of alkali and of cyanide. A knowledge of these reactions, their products, and the factors that influence the rates at which they proceed should be of value in working out the most economical conditions for cyanidation; but at present, much of this knowledge is lacking. This paper is confined to a study of some of the fundamentals of cyanidation. At the start of such an investigation it is necessary to simplify the problem under consideration by eliminating as many variables as possible. The results are then, of course, not immediately applicable to practice, but it is hoped in further work to round out the information and thereby make it of more practical value. For convenience in presentation, the paper has been divided into two parts, one devoted to a study of the reaction between cyanide and gold or silver, the other to a consideration of the factors that determine the rate of dissolution. I. REACTIONS INVOLVED IN DISSOLUTION OF GOLD AND SILVER IN DILUTE CYANIDE SOLUTIONS Ever since the cyanide process for gold and silver extraction was introduced there has been discussion of the equation representing the reactions involved. In undertaking a detailed study of these factors, it was felt that the most logical first step was to determine, if possible, what reactions could theoretically take place when gold and sill-er are dissolved by dilute cyanide solutions. It is possible to determine whether or not a given reaction will theoretically take place by calculating the free energy of the reaction. This free-energy value for any given reaction is the algebraic sum of the free energies of formation of each of the reactants and products, and, if these values are known, the calculation is simple. (A chemical change always involves an energy change and the amount of energy change involved is the factor determining whether a given reaction will take place or how far it will go. In chemistry we consider what is known as the "free energy"; that is, the maximum amount of energy that can be utilized as

Jan 1, 1935

By A. W. Allen

Progress in the art of amalgamation in recent years has been negligible, partly because a copper plate, though it occupies extensive floor space, requires frequent attention and invites theft, is a simple piece of apparatus that gives visible results; partly because the impression prevails that amalgamation is too primitive a process to merit consideration by an up-to-date metallurgist. Both these objections can be overruled. Plates can and will be superseded by more efficient, theft-proof amalgamating units. Improved methods of application other than by settlement or by impact, neither of which is effective for removal of fine gold, will be developed, and the process given wider opportunity. As A. F. Crosse aptly remarked, neglect to utilize amalgamation when free gold can be recovered thus is comparable to the decision of a storekeeper to deal only with credit customers. Usual practice is to follow amalgamation with cyaniding. Rarely is attention paid to the possibility of reversing the order—of extraction of the fine gold first by cyaniding; the coarse, subsequently, by amalgamation. Such a sequence avoids the alleged hazard that amalgamated gold particles may be unacted upon by cyanide, whereas cyanided gold particles are readily amalgamated. Research has indicated, however, that the mercury coating on a gold particle is easily soluble in cyanide solution, probably because such coating is a compound of gold and mercury. Comparative-test results at one plant, of cyaniding a ground concentrate before and after amalgamation, showed total extractions of about 90 and 100 per cent, respectively, indicating high solubility of the mercury-gold particle, if present, or the advantage of preliminary impoverishment before cyaniding, or both. The contention that a loss in residue from an amalgamation-cyanidation plant is occasioned by presence of amalgamated gold that escapes action by solution is not supported by adequate evidence. The function and scope of mercury as an aid to extraction of gold by cyanide is deserving of attention. It is a powerful desulfurizer. To restrict an extractive process to a concentrated product is logical and economical, if preliminary concentration will segregate a high per-

Jan 1, 1935

By G. C. McLachlan

Two papers dealing with Noranda's milling operations have already been presented. The first1 of these covered the initial metallurgical problems connected with the treatment of the ore, while the second2 described the development of the mill from a 500-ton unit in 1928 to one with a daily capacity of 3000 tons less than six years later. At the time the second paper was written the equipment whirh had been installed to bring the mill capacity up to 3000 tons was being tuned into production and for this reason, though each step had previously been tested by a large-scale pilot operation, it was thought advisable to withhold metallurgical data until any starting-up difficulties had been overcome and anticipated requirements fulfilled. These requirements called for an improvement in gold recovery without any lowering of the previous ratio of concentration, and the pages that follow deal with the methods by which this result was obtained. An idea of the character of Noranda concentrating ore will be gained from an inspection of the following mineralogical analysis of the ore treated by the mill during 1933: MineRal Content Mineral ConteNt Chalcopyrite, per cent..... 6.8 Silica and silicates, per cent............ 18.3 Pyrite, per cent........... 22.1 Gold, native and as telluride, oz. per ton 0.15 Pyrrhotite, per cent....... 51.5 Silver, probably as argentite, oz. per tou 0.35 Magnetite, per cent....... 0.5 Thesr figures, which are typical, show that over 73 per cent of the ore treated consists of pyrite and pyrrhotite. Determirnation of the proportion of unrecovered gold associated with each of these minerals was therefore of primary importance in developing a suitable method for improving gold recovery. As pyrrhotite is magnetic, this information was obtained by making magnetic sorting tests on samples of the mill tailing and screening the material thus segregated. This showed that the magnebtic material finer

Jan 1, 1935

By Russell Spry, Paul Schutz

The property of Pioneer Gold Mines of B.C. Limited is in the Lillooet mining district of British Columbia. It is on Cadwalleder Creek, 54 miles distant by motor road from Shalalth, a station on the Pacific Great Eastern Railway. Interests identified with the present company installed a small amalgamation plant on the property in 1924, consisting of a jaw crusher, Bryan mill and amalgamation plates, in which 75 per cent extraction was made on mill feed averaging 1.0 oz. gold per ton, the tailing being stacked for future treatment. That plant was operated until 1928, when the present company was formed and a 100-ton continuous counter current decantation cyanide plant was built. A second unit, having a nominal capacity of 200 tons daily, was added in 1932 and put into operation during September of that year. When handling ore comparatively free from slow-settling material, the combined capacity of the two units is 400 tons, the original plant now handling about 140 tons maximum. Production to date, from Pioneer, has been about $6,500,000, the present monthly production being better than $250,000 from about 370 tons ore daily, the recovery being 97 per cent. During the fiscal year ending March 31, 1934, a total of 112,936 tons ore and old amalgamation tailing was milled, the mill feed averaging 0.7670 oz. gold and the recovery amounting to 0.7422 oz. gold per ton, or 96.77 per cent. Milling costs, including refining and mint charges, during this period, amounted to $1.45 per ton of ore. Since the building of the first unit of the cyanide plant in 1928, direct cyanidation has been employed, no attempt being made to remove coarse gold from the circuit, other than that cleaned up from the grinding mills during relining and from the classifiers, as occasions permit. In the hope of still further increasing recovery, researches are going forward at this time with the view to removing some of the sulfides after primary grinding, the expectation being that selective treatment of this more refractory portion of the ore may hold economic possibilities.

Jan 1, 1935

By Van Dyne Howbert, Fred E. Gray

The Presidio mine of The American Metal Co. of Texas is situated 45 miles south of Marfa, Texas, a town on the Southern Pacific R. R., and lies approximately 20 miles north of the Mexican border. Communication with the railroad is maintained over a state highway. All supplies for mine and mill are hauled in by truck from Marfa and precipitates and concentrates are freighted to the railroad by the same means and shipped to Selby and El Paso, respectively. The mill is at the town of Shafter, 1 mile from the mine and at approximately 350 ft. lower elevation. The ore is conveyed to it by an aerial tramway which requires practically no power on account of the difference in elevation. The mill is a countercurrent decantation cyanide and gravity concentrating plant of 200 tons daily capacity. Coarse and fine crushing are done at the mill. Two neal-by shallow wells in the bed of Cibolo Creek furnish an abundance of water. Power is generated for the mill and town by a Diesel engine plant. Ore Treated The ore is oxidized and siliceous. The greater part contains approximately 16 oz. of silver per ton, but mixed with this are many particles of ore of much higher grade, assaying in many instances 100 oz. or more. In the 16-oz. material there is an almost constant amount of silver which is difficult to recover by cyanidation. The high-grade material contains a much greater proportion of silver which is easily amenable to cyanide treatment. Thus, as the grade of ore becomes higher, the percentage of recovery of silver increases rapidly, under equal milling conditions. The silver minerals contained in the ore are principally argentite and cerargyrite, the former predominating The lead minerals, all of which are argentiferous, are chiefly cerussite and galena, with occasionally a little anglesite. The gold is free; most of the ore contains merely a trace

Jan 1, 1935