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By E.G. Lewis, l.M. Barker

The literature of milling is replete with papers devoted to the subject of ball milling, all of which no doubt have contributed in one way or another to progress in that art. In this paper reference will be made to only a few of the many authors, but the value of the contributions of all who have written on that subject is hereby acknowledged. With a few exceptions the efforts of most students of the subject have been devoted to laboratory investigations of principles. Davis1 was one of the first to report on plant-scale investigations and to present to mill men certain criteria for the guidance of ball-milling practices. His conclusions with respect to the significance of sizing analyses of classifier sands in their relation to the factors of mill speed and ball sizing are particularly referred to. Those conclusions were: 1. If the balls are large or the speed of the mill is high, crowding will appear at the finer sizes in the classifier sands. 2. If the balls are small or the speed is low, crowding will appear at the coarser sizes in the classifier sands. 3. The indications are that best efficiency is obtained when the screen analysis of the sands show a minimum crowding at any size. The last conclusion was qualified by the statement that it had not been proved conclusively. It is surprising, however, that the litera- ture of later years reveals little evidence that millmen have made any serious attempt to apply those criteria. This may, perhaps, be explained by the fact that the average plant-scale ball-milling problem presents so many variables that an investigation of any one of them encounters the problem of control of the others—a problem that often is unsurmountable in a small plant. In a large plant, in which there is a duplication of grinding units in parallel operation, opportunity may be afforded for determining the value of such criteria. Nevertheless, a study of published data from grinding circuits of both large and small plants suggests that either Davis' criteria have been tried and found inapplicable or have never been given consideration. For the purpose of testing Davis' conclusions and with improvement of ball-milling efficiency as the final objective, a test program was initiated in the concentrator of the New Cornelia branch of the Phelps Dodge Corporation early in 1938. The practices of that plant have already been described.2 The fine-grinding units are arranged so that any one of eight units may be operated as a test unit and its results compared with those of the remaining units. All units receive similar feed from a common storage bin, in which the product of the fine-crushing plant is bedded by traveling tripper. The ball mills are all similar in size and operated at the same speeds, and are individually metered. The feeder conveyors of each unit are equipped with Merrick weightometers. The test program as initially outlined proposed investigation of the following:

Jan 1, 1943

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 Fred C. Bond, Walter Maxson

Since the last publication of tabulated results of grindability tests by the authors1 the total number of ball-mill tests made has more than doubled, and rod-mill tests have become increasingly important. Nearly all of the standard closed-circuit ball-mill and rod-mill tests made to date are included in the present tabulation, together with additional information not previously published. Standard Ball-mill Grindability Tests The method of conducting these closed-circuit tests has not been altered. A sample of the ore or other material is stage-crushed in rolls set at 1/16-in. opening with a 6-mesh screen until all of it has passed the screen. The combined minus 6-mesh screen undersize is mixed, sampled and screen-analyzed, and its apparent specific gravity is determined by packing and shaking in a standard container, and weighing. The apparent specific gravity ordinarily is about 60 per cent of the true specific gravity. The unit volume present in the mill .in all tests is 700 C.C. of the packed minus 6-mesh roll product, and the number of grams occupying 700 C.C. is the unit test weight. This weight is placed in the mill dry, ground for the number of revolutions estimated to be necessary, discharged, and screened mechanically in three testing sieves of the mesh size at which the test is to be conducted. The oversize, or circulating load, is weighed, sufficient fresh minus 6-mesh feed is added to bring the total weight up to that of 700 c.c., and the charge is returned to the mill for a second grinding period. All standard ball-mill tests are conducted at 250 per cent circulating load, and the number of revolutions in the mill necessary to obtain this circulating load at any grinding period is estimated from the results of the previous period. The number of net grams of screen undersize produced per revolution of the mill approaches its final equilibrium value after several grinding periods, and this is recorded as the grindability, or relative ease of grinding, of the sample. A cylindrical ball mill, 12 by 12 in. inside, with a smooth lining and rounded corners, is used with a revolution counter Under standard grinding conditions it runs at 70 r.p.m., and contains a charge of 285 iron balls weighing 20,125 grams, ranging from I½ to ¾ in. in diameter. Tests are conducted at the mesh size to which the ore is to be ground in practice, and the capacity- to be expected from a given mill is calculated by comparing the grindability with that of a similar standard ore whose performance characteristics arc known. No satisfactory general formula for convertillg standard grindabilities into corn; rnercial power-consumption values has been

Jan 1, 1943

By Fred C. Bond

The process of comminution by grinding is properly classified as an art, rather than as a science. Like most other operations concerned in ore dressing, or in the treatment of nonmetallic minerals, the mathematical relationships of rock breaking are still obscure, and much disputed. If some basic formula exists, comparable for instance to E = RI in electricity, it has not yet been placed in common use. The absence of such a comprehensive mathematical background undoubtedly is the cause of many inefficient designs and installations, as well as of much poorly oriented experimental work. On the other hand, the mathematical immaturity of the process constitutes an opportunity for a real contribution on the part of those who enjoy mental pioneering. Some of the statements made in any such exploratory work may be little more than opinions, and it is to be expected that some will later be proved untrue; but such an evolutionary development is necessary if we are ever to arrive at the fundamental laws, the discovery of which can change the empirical art into a mathematically exact science. The most significant principle of comminution that we possess is probably Rittinger's law, which states that the work done in crushing or grinding is proportional to the area of the new surface produced. There is an alternative theory, known as Kick's law, which formerly was preferred to Rittinger's but which now is rather discredited. According to Kick, the work done in comminution is proportional to the volume, or weight, of the pieces broken, or to the cube of their diameters, while according to Rittinger it is proportional to the square of the diameters. Careful determinations of size distribution below the limit of sieve sizes1 indicate strongly that under ordinary grinding conditions the amount of new surface area produced is directly proportional to the net power input. Changes in the size ratio between the balls and the particles cause important differences in the proportion of the product that passes a given mesh size, but do not affect the total amount of new surface area; they merely change the distribution of the surface among mesh sizes. The principle of constant surface area is the logical result of Rittinger's law, and it may well have an important bearing on the comminution theories of the future. Formula for Ball Wear Grinding tests have been made in the Allis-Chalmers laboratory for more than 9 years, using a standard charge of mixed balls of different sizes; and a continuous record has been kept of the rates of wear of each size. These results have been combined and plotted in various ways in order to discover the relationship that exists

Jan 1, 1943

By Fred T. Agthe, Fred C. Bond

When some materials are ground dry in a ball mill, a stage of comminution is reached at which the finely divided particles begin to adhere to the balls and to the mill lining. As grinding progresses, a coating accumulates upon the grinding media, which tends to cushion the impacts and thus retard reduction of the material. and finally becomes so thick that all grinding ceases. At this stage, the characteristic noise produced by the grinding media during normal mill operation changes to a dull, muffled sound. In most instances, the formation of the coating marks the practical limit of size reduction. Industrial requirements for fine grinding frequently meet with this obstacle, and the tendency in many commercial operations to grind materials to a higher degree of fineness than formerly makes the solution of this problem an important one. The phenomenon is of far greater importance, therefore, than the limited amount of research and technical discussion devoted to it implies. In order to learn more about the coating of different materials when ground dry to a high degree of fineness, certain laboratory tests were made from which it was found that different materials form coatings at widely different size distributions. It is probable that most materials will coat if they are ground fine enough; the exceptions have inherent lubricating qualities, like coal and graphite. In general, the softer materials tend to coat at coarser sizes than the harder or more brittle materials. Limestone, as an example, will coat more readily than quartz, even though limestones of different- texture and composition exhibit great differences in coating potentialities. Various materials were tested in the laboratory to show the variation in coating qualities. It was found that in most tests quartz must be ground to a fineness that would permit it to pass through 325 mesh before coating became markedly detrimental to the grinding operation. Siliceous rocks, however, tend to coat more readily than quartz. Granite, which is composed essentially of feldspar, quartz and mica, has been found to start coating at about 92 per cent through 200 mesh, and feld-spathic minerals alone usually show a tendency to coat at the same fineness. Barite has been ground in the laboratory to a fineness of 99 per cent through 325 mesh without showing serious coating of the grinding media. Gypsum coats readily. Apatite and phosphate rock usually tend to coat. Hematite usually coats, although when mixed with charcoal it does not do so. In testing the carbonate rocks and minerals, it has been found that burned magnesite, dolomite, and dolomitic limestone coat, whereas calcite and calcined calcite do not coat so readily. It has been found that commercial glass, slate, talc, steatite and coke have little tendency to coat. The relative tendencies toward coating during grinding operations, exemplified by

Jan 1, 1943

By Warren L. Howes

This paper deals primarily with an investigation of ball-mill liners that was conducted by the writer over a period of six years at the Mammoth mill in Arizona. The investigation covered a wide variety of designs of liners in both primary and secondary mills. The comparative results are presented herein as evidence of the extent to which design influenced liner life and mill performance. Flowsheet The feed to the Mammoth mill was a complex, oxidized, gold-silver-lead-molybde-num-vanadium ore with rhyolite, andesite and granite as gangue. Although the ore varied between stopes, the long-term average in character remained substantially the same. Capacity was 560 tons per day.† Fig. I shows an abbreviated flowsheet of the grinding section of the mill. Primary Ball Mill A 3-ft. Symons shorthead crusher in open circuit crushed to 1/4-in. maximum one-way dimension the feed to the 5 by Io-ft. Marcy open-end ball mill. The mill rotated at 80 per cent of critical speed and was charged with 4-in. forged steel balls. Cast balls were used for a few months at a slight reduction in ball cost, but breakage of the large balls reduced the ball size and grinding capacity to a point where the over-all costs suffered out of proportion to the saving in cost of balls. For metallurgical reasons, the finished product of the mill was maintained at minus 8-mesh. This coarse product, plus the very abrasive ore and the absence of fines in the feed, caused abnormally rapid wear of the mill liners. The resultant high operating cost led to the most extensive phase of the investigation. In order to clarify the difference in design of the various types of liners used, Fig. a shows the profiles with the arrangement in which grinding balls of maximum size would lie on the face of the liners. The results with each type of shell liner in the primary mill are shown in Table I. Since most of the testing was done with

Jan 1, 1943

By G. B. Walker, S. A. Falconer, S. J. Swainson, H. H. Vogel

During the past few years much interest and attention has been focused on a relatively new method of ore concentration, which utilizes the principles of sink and float and employs as the heavy medium a suspension in water of a finely ground solid, such as galena or ferrosilicon. Although a relatively recent development, much progress has already been made in applying heavy-media separation processes to a considerable number of ores. Eight plants in this country and abroad are now treating approximately 10 million tons of ore annually by heavy-media separation (sink-float) processes, including lead-zinc, lead, iron, garnet, tin and tungsten. At the annual meeting of the A.I.M.E. in 1941, three interesting papers (unpublished) dealing with heavy-media separation (sink-float) processes of ore concentration as practiced in four commercial units in the United States were presented by Victor Rakowsky, Grover Holt, Elmer Isern and Robert Ammon. These papers gave an excellent exposition of the principles of sink and float, as well as the operating practice in two iron-ore-beneficiation plants, the Harrison and the Merritt, of Butler Brothers, in Minnesota; the Central mill of the Eagle Picher Mining and Smelting Co.; and the Mascot mill, of the American Zinc, Lead and Smelting Co. Augmented by pictorial descriptions and a working model demonstrating the processes, these papers evoked a great deal of interest and discussion. In fact, in reporting the high lights of the meeting in the April 1941 issue of Mining and Metallurgy, Professor Taggart made the statement that " preconcentration by heavy suspension was Miss A.1.M.E 1941 so far as milling is concerned." Although to date the greatest application of heavy-media separation from the tonnage point of view has been for the treatment of lead, zinc and iron ores, these processes have a much wider field of usefulness. In this regard, it is to be noted that recently new heavy-media separation plants for treating cassiterite ore and garnet ore have been placed in successful operation. Moreover, numerous other types of ores have been found to respond well to these processes when tested on a semi-commercial scale, and it is expected that in the near future a considerable number of new plants will be erected. In view of the fact that heavy-media separation processes offer such attractive possibilities, particularly now, when the mining industry is being called on for an even larger production than ever before has been attempted, despite shortages of labor and supplies, it was felt that a description of some of the successful separations that have been worked out during the past year in the Ore Dressing Laboratory of the American Cyanamid Co. on a variety of ores of strategic importance would be of interest. The purpose of this paper, therefore, is to present the essential data relating to investigations of heavy-

Jan 1, 1943

By H. H

This paper describes the milling practice and operating results of the recently installed heavy-media separation plant of Barton Mines Corporation, the world's largest producer of garnet. This pioneer application of heavy-media separation (sink-float) processes for the beneficiation of a nonmetallic ore is unique in many respects, the details of which will be apparent from the following presentation. Characteristics of the Ore The property is on Gore Mountain, 5 miles west of the village of North Creek, New York, and 11 miles by road. The altitude of the mine is approximately 2800 feet. The valuable mineral, garnet, occurs in a surface deposit, the ore body being about ¾, mile long and varying in width from 50 to 300 ft. The garnet, principally almandite, Fe3Al2 (SiO4)3, occurs in a metamorphic rock of uncertain origin. The gangue mineral is principally hornblende, which constitutes from 40 to 80 per cent of the rock. The remainder of the gangue is divided between plagioclase feldspars and hypersthene, with smaller amounts of biotite, apatite and pyrite. The garnet content of the ore body varies from 5 to 20 per cent of the mass and averages about 10 to I2 per cent. The garnet occurs as crystals, mostly imperfectly developed, known locally as "pockets." These crys- tals vary in size from a fraction of an inch to a foot or more in diameter. Occasionally crystals have been found up to 30 and 36 in. in diameter but they average 4 to 6 inches. Nearly every crystal of garnet is surrounded by a rim of coarsely crystalline hornblende. The quarry faces are striking in appearance, showing crimson-red garnet crystals with their coal black rims scattered over a grayish black background. The specific gravity of the garnet is 3.8 to 4.1 while that of the hornblende ordinarily is 3-07 to 3.24. Some specimens of very dense hornblende have been found with a specific gravity as high as 3.40. The garnet crystals are laminated in structure, and readily cleave into flat, tabular pieces with sharp, chisel-like edges. Even when crushed to a very fine size, the garnet retains this flat, sharp, slivery grain shape. This characteristic, together with its hardness and toughness, gives it its value as an abrasive- Former Operations Mining operations have been carried on for 60 years. Until 1923, only the oxidized (soft rock) section of the ore body was mined. The oxidation, which affected the garnet only slightly, made possible the removal of the garnet from the rock by hand after it was blasted down, using small hand picks. In 1923 a mill was erected on the property, and was rebuilt and redesigned in 1928. Before the adoption of heavy-media separation, concentration was effected by

Jan 1, 1943

By E. H. Burdick

The difficulties inherent in table concentration operations as applied to gold, silver, lead and zinc ores, are accentuated in the scheelite mill, which has a flowsheet that is similar in general principles. The narrow "spread" in the specific gravity between scheelite and the usual gangue in which it occurs often makes its clean separation extremely difficult and in some cases impracticable. The problem is further complicated by the extreme friability of the mineral and its inordinate tendency to "slime," particularly where fine grinding is necessary and wet grinding methods are employed. The physical aspect of the occurrence of scheelite in the ores, the kind and character of the rock in which the mineral is present, its hardness, friability and the specific gravity of its constituents, as well as like characteristics of the associated minerals— pyrite, pyrrhotite, sphalerite, and others, all have a bearing on the successful milling of crude ores and the production of a concentrate that is marketable with minimum price penalty or none at all. Most tungsten deposits are considered low grade when the limiting factor of low percentage recovery by gravity methods is borne in mind. The great majority of deposits developed or in process of development carry from 0.4 to 1.0 per cent tungstic oxide. Ore carrying I per cent is considered good grade; 0.7 to 0.8 per cent, fair, and below that figure, low grade. Steady mill feed averaging upward of I .o per cent WO3 is exceptional. Inasmuch as buying specifications demand a 60 per cent W03 content, the mineral content of the ores as mined must be concentrated to at least that degree. A few companies have constructed chemical plants for the treatment of their complex concentrates and low-grade flotation product, but the smaller operator must rely on table concentration, borrowing the tools and to a large extent the methods of his predecessors in the gold, silver, lead and zinc mills. Whether these are the best tools and methods that can be devised is an open question. Except in rare instances, table concentration, however carefully conducted, does not yield a satisfactory final recovery of the mineral content in headings as indicated by chemical determinations of tungstic oxide content. A saving of 60 to 65 per cent is considered fair, and an average 80 per cent recovery, exceptional. Each scheelite ore body is a separate problem. Details of handling that give best results in one case may not be successfully operative at a property on the same contact zone and but a short distance removed. Supplementary treatment of tailings by flotation may be successful in producing a low-grade concentrate of around 15 per cent W03, which is adapted to further treatment chemically at a given property and entirely unsuccessful at another. This problem constitutes another of the unanswered questions. The following paragraphs relate solely to the beneficiation of scheelite ores by table concentration and supplementary methods.

Jan 1, 1943

By Arthur Taggart

Recent jig practice has shown such marked departures from the pronouncements of the textbooks, particularly as to particle size recovered and size range of feed, as to make it desirable to reexamine the mechanism of jig action. This paper presents the results of such a study. The general conclusions of the Paper are: I. A jig bed is a bi-functioned as well as bi-parted body. The upper layer comprises a plastic stream moving slowly in a substantially horizontal direction from feed lip to tail board. It serves to rough out tailing and light middling and to pick up heavy middling and lift it out 01 the jig box. The lower layer acts as the ultimate separating means by absorbing concentrate and rejecting heavy middling. 2. The separating function of the lower layer is performed in three definitely diflerent ways, depending upon the relative sizes of the grains presented to it and those composing it. Experimental The experimental work consisted of close and long-continued visual observations of operating beds in a plunger jig, eccentric driven, and in determinations of the settling rates of various metal spheres through a quartz bed under various conditions of operation. Falling velocities were measured by an ingenious method devised by A. 6. Dorenfeld, a student in the Mining Department at Colum- bia. Spheres of different metallic alloys, 3/8-in. diameter, were cast with a short piece of fine copper wire frozen in to Serve for suspension-A short piece of black cotton thread was looped to the top of the wire to serve as an indicator. The set-up for a test is shown in Fig. I. The thread should be boiled, if necessary, to make it freely water absorbent. The piece of clean plate glass D is supported rigidly at the proper height in a vertical position. The white scale E is similarly supported behind the glass. At the beginning of a test, D is filmed with water by holding it (best with clean rubber finger cots) under running tap water. It is then clamped in approximate position and C, already wet, is laid across it and drawn straight and vertical with the upper end at or near the top of D, and the ball A slightly above the top of the expanded bed. The water film holds the string to the glass. For a test the string is released, its upper end position noted just after the top of the ball becomes submerged, when the corresponding time is read, and thereafter simultaneous readings of position and time are taken as desired. Results of the visual studies of the bed are given at the pertinent places in the following discussion. Results of the settling tests are summarized in Figs- 2 and 3. Definitions The name bed as used herein refers to the entire mixture of solids and water filling the jig box. A layer is a stratum of a bed composed of particles of substantially the same specific gravities. A granular product is long-range when it approximates a crushed or ground product limited as to upper size only; a short-rafzge product is one closely sized. A bed is loaded when operating with continuous feed and discharge of products; it is unloaded when pulsating norma11y but neither being fed nor

Jan 1, 1943

By Keith Leonard Sutherland

This paper is a study of the differential flotation of the sulphide minerals in the presence of salts of silver, lead and zinc. In practice, accidental activation due to these salts is more important than their use as reagents to replace copper sulphate. The general method of investigation has been based upon contact tests, the temperature of 35°C being chosen in conformity with earlier work. Potassium ethyl xanthate and potassium amyl xanthate were selected as collectors and pure sulphide minerals were used. The experimental procedure has been outlined in earlier papers and all solutions were kept carbonate-free.14 Contact, or spreading of an air bubble, at a mineral surface indicates the presence of an adsorbed collector film. Purity of Reagents The xanthates were purified in the usual manner.' Neither the cyanide nor the sodium hydroxide solutions contained sufficient carbonate to give a precipitate with barium chloride solution. The silver sulphate was prepared from pure silver nitrate by evaporation with concentrated sulphuric acid until there was no evidence of brown fumes, This solution was diluted and the difficultly soluble sulphate washed with water so that unchanged nitrate was dissolved. The resultant crystalline powder was pure white. The lead and zinc salts were prepared by dissolving especially pure lead and zinc in C.P. nitric and sulphuric acid solution and the crystals drained. The standard solutions were checked by titration. It was felt desirable to use the sulphate radical wherever possible, but since lead sulphate was insufficiently soluble for the purpose of the experiments, it was necessary to use some other lead salt. A.R. copper sulphate was used without further purification. Results The results are presented in the accompanying figures; the areas of noncontact (nonflotation) are shaded in Figs. 8, 9, 10 and 11; in the remainder they lie to the right of the curve. Zinc Sulphate The curves in Fig. I are to be compared with those for Fig. 2, for which zinc sulphate is absent. This comparison shows that the influence of the zinc ion is usually small. Its influence is more marked, however, for chalcopyrite in the absence of cyanide. The influence of zinc sulphate is also marked for copper-activated sphalerite, for which tests were made only in the "absence of cyanide. The results are of importance in the separation of pyrite from copper-activated sphalerite when zinc sulphate is added in the lead flotation section (p. 204 of ref. I). Sphalerite does not adsorb the collector (i.e., become floatable) under the conditions chosen.

Jan 1, 1943

By Alfonso Rizo-Patrón, A.M. Gaudin

Previous studies of activation in flotation have directed attention to the action of the activator on the mineral to be floated rather than to the relationship of the activator to the collector. The latter phase of the problem, however, seems to have definite scientific, if not also practical, interest. In the investigation reported in this paper, experiments were carried out, largely with quartz as subject, barium as activator, and oleate as collector. The results obtained indicate that a I: I ratio of collector ion to activator ion gives optimum results, and that a 2:1 ratio almost fails to achieve activation and flotation. Yet, a 2:I ratio would have been expected on stoichiometric grounds, had the coating been a normal salt of the activator ion with the collector ion, since barium is a divalent cation and oleate a monovalent anion. To interpret and rationalize the observations, considerations of the crystal chemistry of quartz are helpful. The point of view to which these considerations lead may be of general applicability to systems involving suspensions of solids in liquids; they confirm that an adsorbed coating is inescapable. Apparatus and Supplies The experimental work consisted in barium-ion abstraction tests, hydrogen-ion and hydroxyl-ion abstraction tests, flotation tests, and determinations of the surface of the crushed quartz. The flotation machine was built according to the design of D. W. McGlashan.* It consists of a drill press in which the bit has been replaced by a stainless-steel impellor surrounding a stainless-steel sta-tor, as in the Fagergren laboratory machine. The air intake is controlled by a valve, and the cell consists of a beaker. The quartz was obtained from vein quartz stored in large chunks. It was first crushed to 20 mesh, then sized on a 28-mesh screen. The 20 to 28-mesh size alone was retained for use. This size was freed of coarse iron by passage through a Ball-Norton magnetic separator, bleached with boiling hydrochloric acid to remove residual abraded iron, washed with distilled water until the washings were thoroughly free of ferrous, ferric, and excess hydrogen ion, and stored in covered Pyrex beakers under water until used. The barium was used as barium chloride, Baker's analyzed C. P. The oleate was used as sodium oleate. It was prepared from sodium hydroxide, Baker's analyzed C. P., and oleic acid purified by R. R. de Arellano3 in the laboratories at the Massachusetts Institute of Technology. The purification procedure was elaborated from the recent $researches of Brown and Shinowara.2 It consisted in: (I) saponification of olive oil with potassium

Jan 1, 1943

By S.G. Bankoff

Ince1 proposed that electrostatic attraction between oppositely charged particles was responsible for slime-coating. Del Giudice2 postulated the metathetic formation of a cementing compound. Wark3 suggested that prevention of slime-coating was related to peptization of the slime. In the experiments of Table I the technique employed was essentially that of del Giudice, with the difference that the particle was examined under a film of water rather than dry.4 In general, the polished particle was agitated for 2 min. in a pulp consisting of 12.5 grams of the slime (—200 mesh) and 50 C.C. of distilled water, washed in three baths of distilled water, and examined at 220 diameters with the Leitz Ultropak. Observations of Brownian movement were made at 850 diameters with dark-field illumination. Several of these experiments do not jibe with the metathesis theory. According to published solubilities,5,6 the lead salts of the anions in experiments c through g are more insoluble than lead carbonate, there- fore should prevent the formation of lead carbonate on the galena surface. In experiment i the calcium oxalate, which precumably was on the calcite surfaces, should have permitted the formation of a lead carbonate cement by virtue of its greater solubility. Experiments j through m show that the addition of lime accelerates the deposition of quartz onto a galena surface. The writer is unable to postulate a satisfactory cementing compound, according to the metathesis theory, to explain this effect. These experiments led to the conclusion that the metathetic formation of a cement-

Jan 1, 1943

By Shiou-Chuan Sun

There are several postulations for the mechanism of slime-coating. Incel proposed the electrostatic hypothesis, del Giudice2 suggested the chemical theory; Bankoff3 reported that slime-coating is inhibited whenever the surfaces of the slime particles are ionized sufficiently for Brownian movement to occur, and is facilitated when they are not. These postulations were examined by experiments involving the Burton tube, the cataphoretic cell, and slime-coating. The techniques involved will be described elsewhere in this paper. The electrostatic hypothesis, supported by migration experiments in a Burton tube, was abandoned by del Giudice.2 Experiments of mineral migration in a Burton tube. after the idea of Ince with modification, indicated that this apparatus was inefficient for accurate observation. A cataphoretic cell was constructed. The experimental data, as shown in this paper, enable the correlation and advancing of this hypothesis. Del Giudice's chemical hypothesis considered that slime particles are attached to the galena surfaces by a cement formed as the result of a metathetical reaction between the sulphide and the slime particles. Applying this hypothesis, the calcite slime particles were cemented to the galena surface by the formation of a cementing lead carbonate. In a similar way, lead silicate was considered as the cement of quartz slime coating on galena. Experiments verifying this hypothesis were carried out according to the following procedure: Fresh mineral particles selected from the central part of the broken lumps and examined first under a microscope for ascertaining a clean surface were placed in a small beaker (1.5-in. dia. by 2.5 in. deep) half filled with one kind of slime pulp. The dilution of all slime pulp was 4:I and the particle size of slime was minus 400-mesh. After agitation for 5 min. the specimen was removed by a sharp-end tong and washed gently three times in three separate distilled water baths. It was dried before a small electrical fan and examined immediately under a microscope. A photograph was made of the observation. With reference to the published solubilities,' several of these experiments, which contradict the chemical hypothesis, are listed as following: I. The coating of fluorite slime on the galena surface was light but the coating of galena slime on the fluorite surface was heavy. In a similar way, the coating of quartz slime on the galena was fairly light, but the coating of galena slime on the quartz particle was heavy. According to the chemical hypothesis, using the same constituents and regardless of which is the slime, the density of the coating should be expected to be the same. This, however, as shown above, is not true. Moreover, fluorite (CaF2), having a solubility of 16 mg.4a per liter of water, should not be

Jan 1, 1943

By Arthur F. Taggart, A. W. Thomas, T.C. Fitt

It was noticed early by operators that high recoveries and flocculation of the sulphide minerals were closely correlated in agitation-froth flotation. Later, this readily visible flocculation was found almost invariably to be due to the binding together of the oiled sulphides by minute air bubbles, and is now known to be characteristic of pulps in which at least one of the mineral species is coated with an insoluble collecting oil. In 1930 it was reported1 that in differential flotation a correlation exists between Brownian movement of particles in the pulp and their nonfloatability, and that Brownian movement and dispersion are likewise correlated, whence it would appear to follow that dispersion of a mineral particle in a flotation pulp denotes a particle condition unfavorable to flotation. In 1934 it was postulated2 that Brownian movement, dispersion and nonfloatability all flow from the condition of the surface of the dispersed particles. It was also postulated at that time that the surfaces of dispersed particles are ionized, the ionized compound being a product of reaction between a component of the particle and a component of the pulp, of a mass solubility of the general order of a fraction of a milligram to I 5 to 20 mg. per liter. It was then further asserted, and has since been confirmed by Bankoff,3 that sulphides so conditioned with soluble collectors as to be floatable flocculate without the intervention of air bubbles as binding media. The present paper comprises an inquiry into the nature of the bound and counter ions in zinc sulphide dispersed by sodium arsenate. A part of its findings was mentioned in the 1934 paper above cited.= The tests show that: I. When powdered granular zinc sulphide is immersed in aqueous solutions of sodium arsenate, arsenate ion is abstracted from solution and anchored to the solid surface, while sulphate and lower sulphoxy ions are concurrently displaced therefrom in substantially stoichiometric quantities. 2. The ion counterbalancing the anchored arsenate ion is zinc. 3. Dispersion and Brownian movement of zinc sulphide are concurrently maxima at an arsenate-ion concentration lying between 0.01 and 0.001-molar sodium arsenate. 4. Any condition or reaction that tends. to remove the zinc arsenate coating from the zinc sulphide particles decreases dispersion and Brownian movement concurrently. Experimental Three samples of zinc sulphide were used. Lot I was C.P. zinc sulphide, washed well be~ond absence of chloride, as shown by test with silver ion. Lot 2 was prepared by precipitation from hydrochloric acid solution of arsenic-free zinc, and was washed as lot I. Lot 3 was prepared by heating a portion of lot 2 in absence of air at 1200° to r300°C. for one hour."

Jan 1, 1943

By Arthur F. Taggart, Nathaniel Arbiter

The fact that the floatability of minerals with fatty-acid collectors changes as the pH of a pulp varies was utilized in the early days of flotation, when sulphuric acid was used with oleic acid to float sphalerite and galena. from gangues which themselves float with fatty acids in alkaline pulps. Gaudin1 showed that this difference in floatability is a regular function of the extent of the change in pH. The present paper offers an explanation of the phenomenon, and on the basis thereof sets up recommendations for control of soap-flotation operations. Experimental Parallelism between floatability of a mineral in a given environment and its contact angle in that environment is so well established,2 and the contact angle is so readily and rapidly measurable, that contact angles have been used throughout the experimental work to indicate relative floatability. Experiments comprised contact-angle measurements on a number of representative minerals and metals, and a variety of subsidiary tests designed to check and to amplify the contact-angle indications. Contact-angle measurements were made by the method described in detail by del Giudice.3 Sequence of procedure for determination of the points of Fig. I was: I. Polish specimen. Most specimens yielded zero contact angle after polishing; a few showed a slight "cling." Cling is characteristic of specimens that pit on polishing; it is due to a residue of organic contamination, originally on the particle surface, which persists in the pits. The cling did not change total contact angle after conditioning, and is not, therefore, additive in the upper part of the curves of Fig. I. It may have broadened the bases of the curves for the affected minerals slightly. 2. The specimen was next conditioned in soap solution for 5 minutes. 3. The conditioned particle was transferred, under conditions that precluded surface drying, to an aqueous solution of the pH desired and contact angle determined. 4. The particle was thereupon transferred, again without surface drying, to water. The confirmatory tests will be described at the places pertinent in the argument. Discussion of Results Gaudin and Vincent4 have shown that contact angles with heptoic acid as a collector decrease for a given specimen when the concentration of collector present falls below a certain value. A similar reduction in angle occurs with collector-conditioned particles that are visibly slime-coated, and varies roughly with the extent of coating. Since in the last case the reduction in angle is certainly due to reduction in the proportion of total conditioned mineral surface presented to the bubble, the authors believe that the same condition prevails in the first case cited, and that similar reduction in angle and floatability will occur whenever starvation quantities of collector are present, whether by design or by reason of excessive consumption.

Jan 1, 1943

By Dwight L. Baker, Alexander Knoll

The work herein reported shows that galena in certain organic solutions of fatty acids becomes coated with lead soaps, and that this coating is not only highly water-repellent but is also repellent to certain organic liquids, particularly those of high surface tension; i.e., nitrobenzene, diphenylmethane. Wetting Properties of Galena in Nonaqueous Fatty Acid Solutions When a "captive bubble"I is withdrawn from a polished, plane galena surface under a nitrobenzene solution of stearic acid, the air bubble shows a decided tendency to "cling" to the mineral surface. The contact angle, therefore, was greater than zero, although it was not large enough to be measured quantitatively by the captive-bubble method." When pure nitrobenzene was substituted for the nitrobenzene-stearic acid solution, no clinging of the bubble was observed; viz., contact angle = zero. Although the contact angle developed in air-galena-nitrobenzene-fatty acid solution was small, the organic solvent repellency of the galena surface was great enough to enable good recovery in a laboratory flotation cell2 In Table I are given the results of flotation experiments using several different fatty acids dissolved in nitrobenzene.

Jan 1, 1943

By M. D. Hassiallis

The claim is made in a number of patents1'2'3'4 that some compounds of the class known as aryl sulphides have collector properties. One of these patents generalizes the claim to include all aryl sulphides, whose generic formula is R-S2-R' (where x = 1,2, . . . ), with the restriction that if the aromatic radicals R, R' contain substituent groups these groups may not contain nitrogen or oxygen. Moses, Hess, and Perkins cite as evidence for their claims the results of flotation tests on Anaconda and Miami copper ores using diphenyl sulphide, ditolyl disulphide and dinapthyl disul-phide as collectors. The use of alkyl sulphides as collectors has also been reported5 with the conclusion that the alkyl sulphides are better collectors than the corresponding aryl sulphides. The experimental work cited appears to confirm this contention. In order to test these claims with respect to diphenyl sulphide, a sample, purchased from the Eastman Kodak Co., was tested against Anaconda ore. The procedure followed. was that of Moses, Hess, and Perkins. A sample of ore weighing 500 • grams was placed in a laboratory ball mill. To this was added 220 grams of water, 0.06 grams of commercial diphenyl sulphide (1/4 lb. per ton of ore), and 0.8 grams of lime (3 lb. per ton of ore). The material was ground until 93 per cent passed a 65-mesh screen. This pulp was diluted to 16 per cent solids. A sample of the diluted pulp was placed in a Minerals Separation type of laboratory flotation cell. After a a-min. agitation period, pine oil was added and the froth collected for a period of 15 min. This test recovered 68 per cent of the copper, with a ratio of concentration of 6.8:I. The tailing assay was 0.3 per cent Cu. Moses, Hess and Perkins attained a recovery of 75 per cent, with a ratio concentration of I2:I. Although these results do not compare too well with those of Moses, Hess and Perkins, subsequent tests showed an improvement, as judged by vanning of the tails. It is concluded, therefore, that the patent results are confirmed. Contact-angle Tests In order to study the response of the various minerals, found in Anaconda ore, to commercial diphenyl sulphide, some contact-angle tests were made. Polished particles of bornite, chalcodte, chalco-pyrite, pyrite and quartz were conditioned for 15 min. in a suspension of diphenyl sulphide in water. The concentration of this suspension was 0.284 grams per liter, this being the concentration of this reagent in the ball mill. The conditioned particles were rinsed with water (not rubbed with filter paper or boiled linen) and then tested against an air bubble in the bubble machine, with the following results: born-

Jan 1, 1943

By Arthur F. Taggart, Herbert H. Kellogg, Nathaniel Arbiter

The experimental work herein described is presented in support of the following broad hypothesis: Conditioning of metals and metallic sulphides by amine collectors involves metathetic reaction at the solid surface between the collector and an oxidized metallic compound, to produce a coating comprising an amine-bearing compound of low solubility in the system. The type of reaction is different in acid and in basic solutions; both types may occur simultaneously in near-neutral pulps. Experimental The experiments comprise contact-angle tests with a variety of metals and metallic sulphides and extraction teats on ground chalcocite. Contact-angle tests were made principally on metals. Covellite paralleled metallic copper in amine solution at pH 8.8 (Table 3) and in alkaline water, but maintained an angle of about 70° in Io-3 HCl solution, where metallic copper lost its angle. The tests with anionic collectors (Table I) indicate that the behavior of metals in general is parallel to that of their minerals in anionic solutions. It is believed that this is generally true with cationic collectors also, but the covellite test is a warning against a broad assumption to this effect. All test specimens were mounted in Transoptic.* All tests in conditioning solution were preceded by a test in distilled water; cleaning and polishing were continued in every case until the angle in water was zero. Subsequent transfers into and out of solutions and test cells were made in such a way as to prevent exposure of the surface to air.1 The amine used was primary laurylamine, Armour and Co., AM-1120. It was used in the form of the hydrochloride, obtained by precipitation with gaseous hydrochloric acid from an ether solution of the amine, and purified by two recrystallizations from ether-alcoho1.2 Inorganic and other test reagents were standard laboratory grades. Temperatures were not controlled; the probable range of test-solution temperatures is 650 to 80°F.

Jan 1, 1943

By S. F. Ravitz

In his excellent book on the Principles of Flotation, Warkl makes the following significant statement concerning the theory of flotation: Two questions of first-rate importance must be considered . . . First, it must be decided whether the sulfide minerals require a collector in order that they may float, or whether as has been claimed, they possess an inherent float-ability and need no collector. Second, it must be decided whether the xanthate type of collector can react with or be adsorbed by the unchanged sulfide minerals themselves, or whether, as many claim, reaction with the collector is dependent upon initial oxidation of the mineral surface. In the theory of flotation there are no two questions of greater importance than these. Ravitz and Porter2 presented evidence that galena can be floated without a collector, and even without any reagent, provided oxidation products are thoroughly removed from its surface. They found also that thoroughly cleaned galena floated faster when xanthate was used than when a frother alone or no reagent was used, and that, without a collector, the recovery decreased gradually upon exposure of the mineral to air. Their work, however, has met with considerable criticism.l(127).3-6 This paper is presented to answer the objections that have been raised, and to present additional data that confirin their results. The apparatus used to provide oxygen-free conditions for flotation has been described in detail by Ravitz and Porter. An atmosphere of purified nitrogen was maintained within the apparatus; all water and solutions used were freed of dissolved air, and could be transferred where desired by the use of nitrogen Pressure; nitrogen was used as the gaseous medium for flotation. The flotation cell was essentially a glass cylinder 15 cm. long and 4.6 cm. in diameter. Near the bottom was sealed a fritted glass filter, which broke up the gas into small bubbles, and 6 cm. above this filter was a side arm through which the froth overflowed. The pulp was agitated by a glass impeller, which entered the cell through a mercury seal. For each test 17 grams of galena and 75 ml. of water were placed in the cell, after which the speed of the impeller and the rate of gas flow were adjusted. Water was added gradually during the test to keep the froth level at the proper height. The mineral was prepared and cleaned in the following manner. Exceptionally Pure galena was crushed by hand on a clean bucking board, screened to —I50+ 200 mesh, and deslimed on a 200-mesh sieve with a fine spray of water. It was then boiled on a hot plate for a number of hours with several changes of the desired cleaning solution, after which both the solution and the mineral were placed in the "mineral flask" of the apparatus. The cleaning solution was drained off, and the mineral was boiled with oxygen-free water

Jan 1, 1943