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By G. G. Gunther, C. L. Boeke

(Any discussion resulting from presentation at the Los Angeles Extractive Metallurgy Division Meeting will appear in the November 1953 issue.) I. M. Symonds (Cia Minera de Penoles, Monterrey, N. L., Mexico)—This is a most interesting paper describing zinc deleading operations. Mr. Gunther was kind enough to show me his operation last fall. Outside of the excellent results, I was most impressed by the ease of control. I had expected a difficult operation requiring careful control and supervision, but found one requiring little attention. The only disappointing fact of the separation is the poor copper recovery in the concentrate of the deleading float. The final zinc concentrate still has about 3 pct chalcopyrite (assuming the copper is chalcopy-rite) which adversely affects the zinc grade. If the copper mineral is free, the poor recovery is probably due to the high cyanide concentration. Fortunately, about 75 pct of the copper is recovered before the pulp goes to the zinc circuit. Mr. Gunther's remarks about proper cyanide to zinc sulphate ratios cannot be overemphasized. Although our experience has been mostly confined to the conventional Pb-Zn separation, we have found these ratios most important, and more important in the mill than in the laboratory. The laboratory appears to give optimum results over a wider range of reagent control than the mill, especially in regard to the effect of cyanide. In the mill in handling relatively high grade ores, we usually find that ratios of cyanide to zinc sulphate of 1 to 10 or 20 or higher work best. Where there is a substantial amount of chalcopyrite present, it has been noted that cyanide in the range of 0.02 to 0.10 lb per ton of ore is often beneficial in zinc rejection and possibly in copper recovery in the lead concentrate, while larger amounts, say 0.20 to 0.25 lb per ton, will float more zinc and cause a serious rejection of chalcopyrite. On an ore with 15 to 20 pct Zn content, we have had to use 0.8 to 1.2 lb of zinc sulphate per ton of ore with the above cyanide to obtain optimum results. Sometime ago we made a laboratory study following Parral and Santa Barbara practice on an ore which never had a very satisfactory rejection of zinc in the lead concentrate. The results were not encouraging and a mill test was not run. Since then the study has been reopened using fresh zinc concentrate from the mill in the laboratory instead of one made in the laboratory. A reasonably clean lead float from the zinc concentrate was obtained. It has been checked several times and each time the zinc concentrate made in the mill responds and the one made in the laboratory does not. Although undoubtedly some reasonable explanations can be given, it is presented here only

Jan 1, 1953

By L. L. McMurray

Ilmenite is the most important raw material for manufacture of titanium dioxide.' Industrially, several other products are made from ilmenite, the most important of which are: ferro titanium, ferro carbon-titanium, copper-titanium, titanium carbide and titanium nitride. The production of titanium metal is still in the laboratory stage because of the difficulty of extraction and as yet no important application for the metal has been found. Ilmenite has received considerable attention as an industrial raw material. Imports of ilmenite concentrates for the first nine months of 1941 were 156,737 short tons, the chief source being Travancore, India.2 Domestic produttion of ilmenite has heretofore been confined to Amherst and Nelson Counties, Virginia, where a complex rutile, ilmenite, and apatite ore is mined and treated to utilize all three of these minerals. A recent report3 has described development of the large titaniferous magnetite ore body at Tahawas, New York, where it is expected that 800 tons of ilmenite concentrates, containing 48 per cent TiO2 will be produced daily. Additional domestic production is expected from a large ilmenite deposit recently opened in caldwell county, North carolina. Flotation tests indicate that a high-grade concentrate containing 53 per cent TiO2 can be made from the North Carolina ore. Prospecting of domestic ores in other areas has been reported.' It appears that increased domestic production of ilmenite may well save considerable shipping space so vitally needed in these times. The composition and chemical structure of pure ilmenite is given by Dana as: FeO, TiO2; Ti, 31.6 per cent, Fe, 36.8 per cent, O2, 31.6 per cent. This composition is variable in that some iron or titanium may be replaced, giving a variable iron-titanium ratio. As an example, the iron-titanium weight ratio of ilmenite in Caldwell County, North Carolina, has been determined to be 0.94 (using 97.1 per cent ilmenite concentrate obtained by heavy liquids on minus Iso-mesh ore) compared with theoretical 1.16. No rutile was noted in this ore to account for the low value. This North Carolina ore is free of magnetite, which is a common associate of ilmenite ores. In view of a large potential production from North Carolina, the Tennessee Valley Authority conducted a study of methods of concentration of that ore, of which the results are reported herein. The Ore Five samples of Ore were taken from the deposit at various exposed locations and were mixed for the study and testing. An attempt was made to proportion the amount of weathered and unweathered portions in making the composite sample, so as to approximate actual operating conditions. An examination of representative specimens of the sample showed the following general facts: 1. The black mineral comprising nearly 70 per cent of the ore is ilmenite.

Jan 1, 1948

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 fine (—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 Flotalion 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 frac- . tion 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, 1948

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

WHILE papers on cleaning coal and mining coal were presented at the iron and steel and mining methods sessions, respectively, the first general session on coal was held on Wednesday afternoon. Howard Eavenson of Pittsburgh, Pa., as chairman of the session,* reported progress by the Committee on the Valuation of Coal for Blast-Furnace Coke. A paper on blasting coal effectively and safely in Southern Illinois, by J. E. Tiffany and S. S. Lubelsky, was abstracted and commented on by Dan Harrington, of the U. S. Bureau of Mines. W. J. German commented on some conditions mentioned in the paper as unsafe or bad practices, and added to these some further ex-amples; he made a strong plea for holes to be: drilled parallel to the bedding as the easiest way to determine the proper length or depth to agree, with the depth of kerf cut. Mr. Barron called attention to proper cutting and-drilling and rate of detonation of the explosive used, as effective aids in blasting coal. Another speaker mentioned an odd case where compressed black powder or "pellet powder," had decreased accidents at a non-gaseous mine where permissible explosives had been formerly used; the permissible cracked or shattered the roof, with a resulting high accident rate from falls of roof, and pellet black powder overcame this trouble. Eugene McAuliffe of the Union Pacific Coal Co. told of difficulties in changing from black powder to permissible in Wyoming mines. J. B. Dilworth read a paper on valuation of coal prop-erties, expressing a preference for the method of capi-talizing the earning power of a property. Eli T. Con-ner of Scranton, Pa., with much experience in valuation work, stated that the method was undoubtedly good, but many times failed because of inability to forecast accurately future earnings, and further contended that total valuation -and royalty rates could generally be fixed fairly when based on similar neighboring proper-ties' rates when these had recently been established by a free bargaining. S. A. Taylor of Pittsburgh, Pa., stated that a leasehold value could be fairly established by figuring based on 10 to 20 per cent of the profit resulting from operation. The chairman read a written discussion from Henry Louis of England, called atten-tion to differences in valuation resulting from whether gross or net profit or earnings were used as a basis for capitalizing. John A. Garcia of Allen & Garcia gave a most inter-esting account of coal mining and general conditions in Russia as noted in his recent extensive visit there, which appears elsewhere in this issue. Although agree-ing with most thinking Americans that government operation is incompatible with progress, he showed that mining conditions were far from impossible in present-day Russia. Charles E. Stuart gave motion pictures of parts of the trip, with, his own comments supple-menting those of Mr. Garcia.

Jan 3, 1928

By L. S. Richardson, N. J. Grant

REACTIONS of oxygen and nitrogen at low pressures with titanium have recently been studied by a number of investigators.1-3 Gulbransen and Andrew' noted that the reaction with nitrogen followed the parabolic rate law whereas the reaction with oxygen deviated slightly from this law in the temperature range 300° to 800°C. In the work reported here, commercial titanium (75 A) was used as the test material. Cylinders 2.5 in. long and 0.25 in. in diameter were machined from heavier bar stock. The test pieces were given a metallographic finish, immersed for 30 min in cold concentrated HC1, washed in water, then acetone, and dried with lint-free cloth. Reaction rates were determined in a modified Sieverts type apparatus by measuring the decrease in gas pressure of the reacting gas contained in a constant volume. The amount of gas added could be measured in a calibrated gas burette to an accuracy of 0.01 mm. During the course of a run the temperature never varied by more than 10°C and then only for brief moments. After placing the specimen in the furnace, the system was first evacuated for 12 hr at room temperature, and then flushed with purified argon five times, adsorbed gases being discharged during this period from the glass system with a high frequency spark coil. The flushing and discharging were repeated at 400°C. This rather involved procedure was found necessary after a number of trial runs indicated extraneous effects traceable to the system. Reaction periods up to 2 hr were used, at initial gas pressures of 0.2 to 0.5 atm. Experimental Results Fig. 1 shows the decrease in oxygen pressure for tests at 0.5 atm at various temperatures as a function of the square root of the time. Deviations from linearity are minor and the parabolic rate law is obeyed. Fig. 2 shows the same plot for the nitrogen reaction. A definite deviation from linearity is noted; however, it is probable that the higher initial rates are caused by the presence of small amounts of oxygen contamination, the initial faster rate changing to the slower rate after about 5 to 10 min. Calculations of the rate constants were made on the basis of the latter portion of the curves. The parabolic rate law constants calculated from these curves are shown for oxygen and nitrogen in Fig. 3. In spite of some scatter the average curves are quite definite. Changes in gas pressure of the order of 20 pct did not result in a measurable change in the rate law constants. The activation energy for the oxygen reaction was calculated to be 47,400 cal per mol (above 700°C), which is not in agreement with the value quoted by Gulbransen and Andrew' for lower temperatures, their value being 26,000 cal below 600°C. The activation energy for the nitrogen reaction was calculated to be 45,400 cal per mol above about

Jan 1, 1955

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 fine (—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 Flotalion 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 frac- . tion 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, 1948

By C. G. Dunn, F. W. Daniels, M. J. Bolton

J. P. Nielsen—The data that Dr. Dunn and his associates have been obtaining are welcome checks on the theoretical aspects of grain boundary energies. With reference to the comments on the validity of the inter-facial tension concept, I should like to say that I have been having considerable difficulty myself in untangling the confusion between "interfacial tension" and "interfacial energy." The confusion however resolved itself for me when I learned that "interfacial tension" for solids, or at least crystals, is used with two distinct meanings. One meaning12. ' "hat is implied for "interfacial tension" is the work necessary to produce or increase the surface of the solid in question by a unit area, temperature and pressure held constant. This comes from the somewhat surprising but simple fact that surface tension and surface energy in the case of liquids are identical quantities. This synonymity has carried over to crystals, where it should be kept in mind that the tension connotation has meaning only by analogy with liquids and that no real stresses are being referred to. The only reason that there is apparently a set of stresses acting at a grain boundary junction is the optical illusion that liquid interfaces are being observed for the grain boundaries. The other meaning3,14,15 for the term has to do with actual states of stress in the surface of a material as would be measured by a system of forces applied to the surface to equate the surface stress state with that in the body of the crystal. J. B. Hess—Since the authors have proposed that the surface tension concept should be discarded in order to deal with the general case of interface energies in solids, their attention should be called to a recent paper by Gurney." The latter has shown, from a thermodynamic argument, that surface tension is a valid concept in solids. In fact, Gurney has rejected the idea that surface tensions are merely mathematical fiction and, instead, has given an interpretation of their physical reality. Finally, he has concluded that, as long as appreciable atomic migration takes place, specific surface energies and surface tensions must be equivalent in solids as well as in liquids. Accordingly, the authors' eqs 2 and 3 can be written with equal accuracy in terms of interface tensions, simply by replacing each E,! with its numerically and dimension-ally equivalent Interfacial tension ?,,. If the interfacial tensions (or specific energies) are independent of interfacial orientation, as is true in liquids, then the general equations that define the geometry at equilibrium of the common junction of three interfaces reduce to eq 1. However, neglect of the effect of boundary orientation is never completely justified theoretically' in dealing with crystalline solids; hence, use of eq 1 in such cases must always be considered as an approximation, though clearly a reasonable one for many purposes.1,2 At the same time, one should not be surprised that the assumption that interface tensions in solids are free from orientation

Jan 1, 1951

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 Si02, and a very fine (-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 fraction 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.

Jan 1, 1945

By D. H. Baldwin, R. E. Reed-Hill

DURING the course of experiments involving oxygen equilibrations with a high-purity Pd-5 at. pct Rh alloy, the appearance of a subscale was noted. Most of the heat treatments in a pure oxygen atmosphere were performed at 900°C. The presence of the subscale was noted when the oxygen partial pressure was in excess of approximately 95 mm, up to 1 atm, the highest pressure used. According to available thermodynamic information' on the free energy of formation of Rh2O3 (the only reliably reported solid oxide of rhodium), this oxide should not be stable under these conditions, nor, of course, any oxide of palladium. Extraction of the subscale from the matrix was affected by treatment with aqua regia, and the resulting X-ray diffraction powder pattern is shown in Table I. This pattern is not that of Rh2O3, nor that of any known rhodium or palladium oxide. It can be indexed on a hexagonal lattice with a. = 5.22Å and co = 6.0Å. In addition to this unknown material, there was a weak Rh2O3 pattern. An X-ray fluorescence analysis of the powder gave 3214 palladium counts per sec and 5381 rhodium counts per sec, thus indicating the likelihood of a double oxide of palladium and rhodium. In view of the fact that the above result was obtained on a single sample, it is perhaps best not to insist upon the above ratio of about 0.6, but possibly to tentatively assume 0.5 or 1/1. The small amount of Rh2O3 in the X-ray pattern might have occurred on cooling, and it seems possible that the double oxide, below some temperature level, is not as stable as Rh2O3. To examine this point, some of the extracted double oxide was heated on a sheet of pure palladium in air at 900°C, and allowed to furnace-cool over a period of several hours. The X-ray diffraction pattern of the powder showed approximately the same intensity of Rh2O3 and the "hexagonal" oxide as before, but, in addition, a rather faint pattern of another crystalline species made its appearance. This finding again suggests partial transformation of the major (double) oxide to other oxides on cooling from 900°C. Application of the phase rule shows that only one equilibrium oxide (subscale) could have been present at temperature. Vacuum-fusion, oxygen analysis of the extracted subscale showed 7.7 ± 0.7 pct O. Combining this information with that of the X-ray fluorescence analysis suggests the formula PdRhO. This compound should have an oxygen content of 7.07 pct, which is within the range of error of the oxygen analysis. However, until a more careful stoichiometric study is made, it is suggested that the formula be written

Jan 1, 1965

• In 1949 the United States imported 7,400,000 tons of iron ore; Chile, Sweden and Canada, in that order of importance, supplied over 80 pct of this amount. U. S. imports have increased from 3 pct of the total supply in 1940 to 8 pct in 1949. • Mica has been successfully synthesized by scientists of the National Bureau of Standards. quartz, magnesite and bauxite, plus a fluorosilicate compound to act as a crystallizing agent, are heated to 2500°F in a platinum-lined crucible and as the furnace cools mica crystals grow. The key to parallel growth to make sheets is in precision control of temperature. • Inland Steel Co. of Chicago has taken an option to lease from Steep Rock Iron Mines, Ltd., of Canada -- a large undeveloped acreage in the vicinity of Steed Rock Lake, Ontario -- for the purpose of exploring and developing a new iron ore mine. The exploration program is expected to begin at an early date. •A 20-yr test conducted by the U. S. Bureau of Mines with the cooperation of Cleveland-Cliffs indicated that chemically treated timbers last from 2 to 3-1/2 times as long as untreated ones set in the same passageway. Of the three reagents used, zinc chloride gave the best result -- 13.3 yr as compared to 3.8 yr for untreated timber. •Senator Pat McCarran charged that President Truman used a "shotgun approach" to the taxation problem when he accused the mining industry of enjoying excessive depletion exemptions when actually mining taxes should be lowered. He introduced to the Senate a report of the National Advisory Council -recommending a decrease * The country's first graduate program of research and instruction in conservation of natural resources will begin at Yale in September. The Conservation Foundation is supplying $20,000 a year to finance the program. •Felix E. Wormser urged that adequate tariff protection should be provided to offset effects of devaluation on the domestic mining industry in an address before the Colorado Mining Association. He advocates tariffs rather than subsidy legislation, such as S. 2105, for the protection of the lead-zinc miners because the latter would promote inefficiency and "impair our priceless free market." •"It may be startling to realize that for the world's white population the per capita requirements for minerals have multiplied 30 times in 30 yr, or that more minerals have been mined in the last 40 yr than in all prior history." -- Evan Just, in "Mineral Depletion and Metal Supply." •The National City Bank in its monthly letter states that both management and the unions concede that there are too many miners trying to make a living out of the industry for its present market. •On Feb. 3 it was reported that 6000 Anaconda employes in Chile quit jobs in sympathy with striking telephone and electric workers. The government has ordered them back to work on penalty of discharge. It appears that the walkout will not be prolonged in view of the government stand.

Jan 3, 1950

Samples of the feed, underflow and overflow mediums from dense medium cyclones operating at low separation densities in eight commercial coal washeries were sized and analysed, to obtain comparative cyclone classification performance curves for the magnetite, shale and coal components in the circulating medium. The resulting component classification curves indicated that the dense medium cyclones hydraulically classify the magnetite and the shale to the underflow with a Stokesian size and density relationship at these low medium densities, ie the shale curve was shifted parallel to and appropriately coarser than the magnetite curve because of the lower density of the shale. However the lower density coal reverse classified to the overflow (ie away from the cyclone wall) with a similar Stokesian relationship. By correcting the magnetite and shale classification curves for the bypass inefficiency to underflow, and similarly correcting the coal classification curves for the bypass inefficiency to overflow, the corrected classification curves for the magnetite, shale and coal were reasonably parallel (considering that the coal has a range of densities). Using a value of five for the density of the magnetite, the displacement of the shale and coal curves corresponded to densities of 2.27 and 1.38 respectively for one circuit, although the data was not as good for the other circuits. This reverse classification mechanism was confirmed in a 140 mm diameter laboratory dense medium cyclone circuit using low density (1.20 - 1.30 RD) tracers, sized from 0.25 to 2 mm. These classification performance curves were corrected for bypass ineffiency (as above). The corrected curves were parallel and displaced according to tracer density, even though the lowest density tracers were reverse classified to the overflow. The data indicate that the rates of classification of all particles could be described by the same Stokesian relationship, regardless of the direction of travel, except for a narrow band at the partition density. Particles heavier than the partition density classified to the underflow, particles lighter than the partition density reverse classified to the overflow and particles identical to the partition density were not classified at all. Consequently it should be possible to simulate partition in dense medium cyclones, operating under free settling low density conditions, with a simple cyclone classification model, provided the partition density can be accurately calculated from, or correlated with the cyclone feed, underflow or overflow pulp densities. The tracer partition performance in the laboratory cyclone was an inverse function of the tracer particle size, as proposed by King and Juckes (1984) for medium/coal ratio in low density medium systems. Their sized coal data was parallel, with lower partition values due to a higher energy cyclone. Partition data with similarly sized tracers (Scott, 1988) showed a parallel shift to higher partition values due to the separate effects of higher viscosity medium and a larger diameter lower energy Cyclone.

Jan 1, 1993

By J. W. Borough

THE electrical conductivity of pure copper is markedly decreased by small amounts of impurity in solution. The magnitude of this effect has been very carefully determined by numerous investigators who studied a wide variety of impurity elements. Much of this work is summarized in an excellent review by Pawlek and Reichel.' The case of zinc impurity in copper is an exception to the above in that there has been no well-documented study of the effect using high-purity starting materials. The values for the effect of zinc on conductivity, which are usually taken from unpublished work by Skowronki, indicate that zinc in low concentration has no effect whatever in lowering the conductivity of pure copper. This effect, if true, is unusual since it is generally known that even in lowest concentration, impurities exert an effect on conductivity which is proportional to the amount dissolved. It is more reasonable to suspect that in the original work on the effect of zinc some of the zinc was oxidized out of solution during specimen preparation. The following experi- and calculated d-spacings based on the unit cell dimensions of Baenziger et al. Since the single crystal studies of Baenziger et al. were limited to (hk0) and (hk 1) data, it was not possible to Compare all the intensities of the powder and single crystal patterns. However, the strongest reflections of both studies, the (321) reflection, agree very well when the appropriate multiplicity factor is used. Good agreement was also found in a number of other reflections of lesser intensity. Despite the precautions taken in annealing the U6Fe powder, an appreciable amount of UO, was detected in the powder pattern after heat treatment. The powder pattern reported by Groganoand Clews is given in Table I. Except for the 3.15A line, which is the strongest line of UO,, their pattern, as far as it goes, compares favoEably with the data from this study. Gordon and Kaufmann have reported a diffraction powder pattern purported to be U, Fe but it bears very little resemblance to the patterns of Table I. ments were carried out to redetermine the effect of zinc on conductivity using high-purity starting materials and processing conditions capable of producing oxygen-free alloys. Materials used in the experiment were ASR 99.999 pct Cu and Cumingo 99.999 pct Zn. Four 1 lb melts were prepared with identical procedure in argon atmosphere with crucibles made from Speer No. 580 graphite. The compositions were 0.0, 0.1, 0.3 and 1.0 pct Zn. Standard No. 14 wire (0.064 in. diam) was made from these melts as follows. The 1 pct Zn sample was first reduced 94 pct by cold swaging with five annealing treatments of 800o for 10 min in hydrogen between swagings, and then reduced 94 pct to the

Jan 1, 1962

By B. L. Averbach

THE rolling process may be considered as a case of a nonhomogeneous plastic flow. In such a heterogeneous deformation there is no direct general solution, and the plastic deformation varies from point to point as a function of the coordinates. It is practicable to determine these plastic strains only at the conclusion of the rolling process, and the local strains can be studied by observing the deformations produced in a suitably placed grid system. Strains at the surface of a bar after rolling have been reported by MacGregor and Coffin,' but the strain distributions within the bar have not been previously observed. Siebel² has investigated the plastic deformations resulting from wire-drawing by splitting the wire along its axis, milling a grid coordinate system on the inner plane surfaces, and binding the .wire together so that it would pull through a die as a single unit. This method was possible because of the rotational symmetry of the die. In the rolling process, however, such a system was not readily applicable. This paper describes another method of including a grid system, and reports some preliminary data on the plastic rolling strains within a square bar. Experimental Procedure 2.1 mm wide (144 network squares per sq in.) was punched from a thin lead sheet with a steel die and supported in a brass mold by thin copper wires. Pure tin was then poured around the grid to form a solid bar, with the network securely imbedded at. a given position. This bar was then machined to a square 15.2 mm (0.60 in.) wide, and then radiographed. The lead grid was quite adherent and sufficiently ductile to follow the deformation of the bar faithfully. The network lines also remained sharp enough to maintain a high radiographic contrast, and the tin bar, with the grid included, could withstand considerable deformation at room temperature without splitting at the interface. In order to fill the mold, it was necessary to cast the tin at 260-280°C and during pouring the lead grid was supported at short intervals to prevent warping. Some shrinkage cavities were encountered, but only bars which were free of shrinkage in the network region were used. This method is similar to the one employed by Steinberg" in an investigation of the strain distribution in a tensile specimen. Before rolling, the machined bars were radiographed in two directions to obtain accurate initial dimensions of each square and to observe whether the grid was straight and correctly positioned. The rolling was performed in a small hand mill with 2 in. diam rolls at room temperature, and a 20 pct reduction based on the original height was employed. The rolls were clean and no lubricant was used. Halfway through the bar, at the center of the network, the rolls were reversed and the bar extracted. These bars were then radiographed again

Jan 1, 1951

Discussion of the paper of G. P. Hulst, presented at the Salt Lake meeting, August, 1914, and printed in Bulletin No. 92, August, 1914, pp. 1865 to 1871. L. S. AUSTIN, Salt Lake City, Utah.-One question that I would like to ask is in regard to the sampling kettle which stands beside the softening furnace. How is the sample taken or melted? G. P. HULST.-The sampling kettles in question are of 45 tons capacity and are fired with coal. The lead bullion comes in on a high line in car-load lots of 30 to 40 tons. The entire lot is trucked from car, weighed over scales and thrown into the sampling kettle, which has been previously cleaned. The kettle is fired and the bullion melted, then heated up until no frozen bullion' remains in the .bottom or adheres to the sides of the kettle. The kettle is scraped clean, sides and bottom, and the wet dross is skimmed Doff clean into molds. The kettle is stirred thoroughly during the period in which 24 to 30 samples of approximately ½ assay ton are taken. These samples are taken in a long-hand loci iron mold, providing for taking six to eight "gumdrops." The mold is inserted and heated to the same temperature as the molten metal, and gumdrops are clipped out and cooled in the mold by dipping 'the bottom of. the mold into Water. The samples should be free from fins. The gumdrops represent the contents of the kettle, and in assaying, they should not be clipped, but weighed up and the result computed. The dross bars are weighed and sawed according to old hammer and punch sample template. The sawdust represents a sample of the dross. In eases of high gold in the bullion there is a slight correction in the assay. This method of sampling was developed at the Omaha plant of the American Smelting & Refining Co., W. T.. Page, Manager, in 1903 or 1904, for adjusting differences in checking smelter sampling. L. S. AUSTIN.-The base bullion which you treat is very clean. It has been remelted, and skimmed before shipment. How rapidly can you get it through the softening furnace, and how does it compare with ordinary base bullion? G. P. HULST.-Twenty-four hours is the softening limit on these charges. In other words, it is charged into the furnace, heated up, and the first and second skimmings are taken off, and it goes into the kettle the next day; that is, 24 hr. elapse from the time the bullion is charged to the time it is in the kettle. L. S. AUSTIN.-It seems to be a long time to hold such a pure bullion. I suppose, though, it comes around conveniently so that you have a time for all the other operations of refining. Isn't that the case? MR. HULST.-Every refinery is based on those principles.

Jan 11, 1914

By B. L. Averbach, M. Cohen, G. P. Conard

IT has been frequently observed that, when metal crystals are bent and annealed or when they are bent at elevated temperatures, the asterism of the Laue spots is split discontinuously into tiny intensity maxima. This finding indicates that segmented crystallites or subgrains are produced, which are relatively undistorted within themselves but which differ slightly in orientation from their neighbors. The following viewpoints have been put forward concerning the nature of this segmentation process: 1—Crussard' has described the phenomenon as "re-crystallization in situ." According to this mechanism, the deformed lattice recrystallizes on heating into an aggregate of comparatively strain-free subgrains separated from one another by low-angle boundaries and having nearly the same orientation as the original crystal. This process differs from the classical type of recrystallization in that the latter involves the formation of grains having quite different orientations from that of the mother crystal. 2—A similar but more detailed picture has been advanced by Cahn' who adopted the term "polygonization." In this interpretation, the plastic bending of lattice planes results in an excess of dislocations of one sign, but at suitable temperatures these dislocations migrate along slip planes and collect in localized regions to form an array of low-angle boundaries. Concurrently, the lattice segments between the boundaries lose their curvature and elastic strain. 3—The "cell formation" concept of Wood and co-workers: unlike the two hypotheses cited, postulates that the segmentation of the lattice is basically a mode of deformation and is not an annealing phenomenon. Cell formation appears to compete more effectively with respect to the normal slip process as the deformation temperature is increased and as the strain rate is decreased. The present work was performed on 3.2 mm diameter 99.99' pct Zn single crystals, grown from the melt in a gradient furnace. The major impurity was 0.003 pct Fe. The crystal orientations ranged from those with basal plane parallel to the rod axis to those with the basal plane almost perpendicular to the rod axis. The specimens were bent on templates to effective radii varying from 14.2 to 1.3 cm at the temperatures from —196" to 100°C. In each case, the axis of bending was parallel to the basal plane. Subsequent annealing was carried out at temperatures from —196" to 400°C. Back-reflection Laue pictures were taken on the convex surface of the bent specimens, before and after annealing. This procedure was found to yield better resolution of the detail in the diffraction spots than did the previously used Laue transmission technique. Some X-ray pictures of rods bent at —196" and —78°C were taken at these respective temperatures without intermediate warming to room temperature. In addition, bent crystals were acid cut" parallel to the basal plane, and double-crystal spectrometer rocking-curves were obtained from the etched (0001) face before and after increment an-

Jan 1, 1954

The meeting was called to order in the Albany hotel, with the President, John B. Marks, in the chair. At the request of the Secretary, the chairman brought before the Institute the question of a reorganization of the finances and system of conducting the Institute, explaining that, although the Institute is in good financial shape and the meetings are of great interest and are attended by a large and serious minded membership, the Institute is getting so large and of such value to the operators that it should be taken over by the operators, conducted by some man elected by and from the operators, and its financing put on a definite basis. At present, it was explained, the Secretary, not a coal operator nor interested in operating, arranges and conducts all meetings and finances the Institute from three sources: the very low dues, the advertisements published in the Proceedings, and by direct solicitation of contributions among the supply and machinery houses. Mr. James Dalrymple spoke vigorously on the need of having the Institute entirely free from any taint of commercialism. Upon motion by W. D. Brennan, seconded, a committee of four, one to represent each State, was voted. Appointment of this Committee was deferred temporarily. The reading of the minutes of the previous meeting was then called for, but upon statement of the Secretary, that the minutes were published in Volume 2 of the 1925 Proceedings, they were dispensed with. The Secretary-Treasurer's report was made informally inasmuch as the last report had not yet been audited. In brief, the Secretary reported on a cost of approximately $1,600.00 a year to publish and send out the Proceedings, an expense of approximately $1,800.00 to care for the Denver meeting, and an expense of approximately $1,200.00 to care for the summer meeting. The Secretary's salary of $25.00 a month has not been collected, but a certain portion of this has been used for stenographic expense. The Secretary asked for expression from the floor regarding the advisability of continuing the publication on the present elaborate plan. Mr. Gibson, Mr. Marks, Mr. Whiteside, Mr. Littlejohn, Mr. Dick and others spoke positively on the value of the present form of the Proceedings, and urged that no changes be attempted in this. Upon motion of Holbrook Mahn, it was moved, seconded and carried that E. H. Weitzel and W. F. Murray be made life members of the Institute in recognition of their services in the organization of the Institute, placing them with Floyd W. Parsons as the original organizers of the Institute. Mr. Murray spoke briefly in acknowledgment of the courtesy. Mr. Weitzel's words are included in the discussion A letter was read from George B. Pryde relative to the present emblem of the Institute. Upon motion by Mr. C. W. Sinclair, seconded by Mr. Dalrymple, it was moved that the consideration of a new emblem be

Jan 1, 1926

By Maurice Rey, H. Brevers

Through circumstances connected with the war, the senior author lost his records, therefore it has been impossible to include numerical data in this paper. The arsenical quicksilver ore investigated had been roasted, with poor metallurgical results. The vapor-tension temperature curves of mercury and arsenious trioxide are similar, and the arsenical compound hampers the coalescence of mercury drops in the condenser and is the cause of large stack losses. The ore was a gray limestone carrying small amounts of carbon and mineralized with cinnabar and two arsenic minerals, realgar (As2S2) and arsenopyrite (FeAsS). The proportion of realgar often exceeded that of cinnabar; the proportion of arsenopyrite was smaller. The grade of the ore varied between 0.8 and 4 per cent Hg. The problem was to make a high-grade mercury concentrate, as free from arsenic as possible. The water used throughout the testing was hard, having a pH of about 8. Flotation of Realgar Realgar showed a very strong tendency to float. It formed a film at the surface of the pulp and floated in abundance with only pine oil. Therefore an attempt was made to float the realgar before the cinnabar, but this was not very successful; the percentage of mercury in the realgar concentrate could never be brought below 2 or 3 per cent. Cinnabar slimed easily and floated with pine oil, so that some of it always accompanied the realgar. There was also the question of the cinnabar-arseno-pyrite separation. On further investigation it was found that realgar can be floated not only with pine oil but even better with a combination of hydrocarbons and pine oil. Washing the ore with ether revealed that it contained hydrocarbons, which helped to float the realgar. In this connection it belongs to the same class as carbon, sulphur and talc. It can be floated also with a xanthate, when activated by a heavy-metal salt. The conditions favoring the two types of flotation are opposed, as activation by a copper salt facilitates xanthate flotation (in fact, is even necessary to it), whereas it hinders pine oil and petroleum flotation. One type of flotation can be termed non-polar and the other polar, a distinction that has been stressed in a previous paper.' Depression of Realgar and Flotation of Cinnabar Many chemicals were tested in an attempt to float the cinnabar and depress the realgar. Finally starch rendered soluble with caustic soda was tried, also several grades of commercial soluble starch, and dextrin was found to be the best and the most convenient reagent. Several of these starch preparations have a strong flocculating effect on the pulp, which is a distinct disadvantage. Dextrin, with its low flocculating power, is excellent. It is noteworthy that starch preparations are also depressants for carbon and talc, so that the fact apparently has a general

Jan 1, 1943

By L. L. McMurray

Ilmenite is the most important raw material for manufacture of titanium dioxide.' Industrially, several other products are made from ilmenite, the most important of which are: ferro titanium, ferro carbon-titanium, copper-titanium, titanium carbide and titanium nitride. The production of titanium metal is still in the laboratory stage because of the difficulty of extraction and as yet no important application for the metal has been found. Ilmenite has received considerable attention as an industrial raw material. Imports of ilmenite concentrates for the first nine months of 1941 were 156,737 short tons, the chief source being Travancore, India.2 Domestic produttion of ilmenite has heretofore been confined to Amherst and Nelson Counties, Virginia, where a complex rutile, ilmenite, and apatite ore is mined and treated to utilize all three of these minerals. A recent report3 has described development of the large titaniferous magnetite ore body at Tahawas, New York, where it is expected that 800 tons of ilmenite concentrates, containing 48 per cent TiO2 will be produced daily. Additional domestic production is expected from a large ilmenite deposit recently opened in caldwell county, North carolina. Flotation tests indicate that a high-grade concentrate containing 53 per cent TiO2 can be made from the North Carolina ore. Prospecting of domestic ores in other areas has been reported.' It appears that increased domestic production of ilmenite may well save considerable shipping space so vitally needed in these times. The composition and chemical structure of pure ilmenite is given by Dana as: FeO, TiO2; Ti, 31.6 per cent, Fe, 36.8 per cent, O2, 31.6 per cent. This composition is variable in that some iron or titanium may be replaced, giving a variable iron-titanium ratio. As an example, the iron-titanium weight ratio of ilmenite in Caldwell County, North Carolina, has been determined to be 0.94 (using 97.1 per cent ilmenite concentrate obtained by heavy liquids on minus Iso-mesh ore) compared with theoretical 1.16. No rutile was noted in this ore to account for the low value. This North Carolina ore is free of magnetite, which is a common associate of ilmenite ores. In view of a large potential production from North Carolina, the Tennessee Valley Authority conducted a study of methods of concentration of that ore, of which the results are reported herein. The Ore Five samples of Ore were taken from the deposit at various exposed locations and were mixed for the study and testing. An attempt was made to proportion the amount of weathered and unweathered portions in making the composite sample, so as to approximate actual operating conditions. An examination of representative specimens of the sample showed the following general facts: 1. The black mineral comprising nearly 70 per cent of the ore is ilmenite.

Jan 1, 1948

By W. R. Aufricht, E. H. Koepf

The theory, measurement, and application of capillary forces in reservoir rock have been treated ex-tensively in the various petroleum publications.1,2,3,4 These forces are of prime importance in oil production, and data on capillary properties are among the most important tools used in the study of reservoir mechanics. The principal application of measured capillary pressure data by the production and reservoir engineer is in the determination of the initial distribution and mobility of fluids in the reservoir. The distribution refers to the magnitude of the oil and interstitial water saturations under capillary equilibrium conditions and to their variation throughout the reservoir as a result of changes in rock properties and nearness to free water. The magnitude of the water (or oil) saturation, as well as the porosity, is required in volumetric calculations of oil in place. In low permeability reservoirs, where long transition zones are common, the magnitude of the oil content, even below the depth interval where commercial rates of flow of oil can be obtained, must be evaluated since this oil contains energy available to the production of the remainder of the reservoir. The mobility of the water phase is of particular importance in water-flood calculations since mobile water may condemn what would otherwise be a successful water flood. In reservoirs with predominantly small pores, high immobile water contents are possible. Conversely, reservoirs with predominantly large pores may contain mobile water even though the interstitial water contents are relatively low. This presentation reviews the distribution and mobility of interstitial water contents as determined from capillary pressure data and shows typical data for various types of carbonate reservoirs. A discussion of the variations found in different types of carbonate reservoirs is given. DISCUSSION Interpretation of Laboratory Data Fig. 1 is a typical laboratory capillary Pressure curve where water saturation as Per cent of Pore space is plotted vs capillary Pressure (psig) for an air-water system. This par- ticular curve was obtained by measurement on a sample of San Andres dolomite with intergranular-type porosity. The sample studied had a permeability of 10.0 md and a porosity of 18.8 per cent. The capillary pressure-saturation relationship illustrated is an inherent property of the rock (a function of the size and distribution of the pores) and represents the ability of this water-wet rock to retain water against the pressure differential exerted by a non-wetting fluid (oil or gas) to remove it. In the laboratory a known pressure differential is exerted from a pressure source; in the reservoir the pressure differential is controlled by the density difference between the hvdrocarbons and the water. The laboratory capillary pressure values may be converted into terms of equivalent height of water column using known values of reservoir oil and water density and measured or average values of interfacial tension

Jan 1, 1958