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By Walter Crafts, C. M. Offenhauer

In a previous study of the carbide phase of chromium steels, it was shown that chromium carbide (Cr7C3) is 2 more stable carbide than cementite (Fe3C) at tempering temperatures above about 500°C. in quenched steels containing from about I to 7.5 per cent chromium. Below this temperature the carbide phase was found to consist of cementite in all of the steels examined. In the present investigation it was found that a similar change in the carbide phase takes place in molybdenum and in chromium-molybdenum steels at approximately the same tempering temperatures. The approximate ranges of occurrence of the alloy carbides Cr7C3, Cr4C, and Mo2C have been determined in steels containing up to 5 per cent chromium, I per cent molybdenum and 0.60 per cent carbon. The experimental steels were made in small high-frequency furnaces from Armco ingot iron, low-carbon ferrochromium and calcium molybdate and were poured into 2-in. ingots, which were forged to I-in. round bars. Sections of the bars were heated to the carbide-solution temperature and cooled rapidly to induce austenite transformation at relatively low temperatures. The steels were subject to some segregation, therefore comparatively high temperatures were necessary to dissolve all of the carbides. The microstructure of the quenched specimens was examined to verify the belief that the carbides had been dissolved, and also to determine the nature of the nonmartensitic structure of incompletely hardened steels. Ferrite and pseudo-martensite were present in some of the specimens, but all specimens were quenched at such a rate that pearlite was not formed, in order to ensure the formation of the carbides at temperatures lower than about 500°C. It had been found previously1 that in chromium steels the chromium carbide could be produced by transformation of austenite in the pearlite range above 500°C., and, in order to start the tempering treatment with the carbide present as cementite, the absence of pearlite was considered to be essential. The specimens were tempered for 64 hr. to permit the formation of the stable carbide. After tempering, the specimens were submitted to microscopic and X-ray examination. The carbides were separated either electrolytically in a 5 per cent HCl electrolyte or with an acidified copper-potassium chloride solution. The crystal structure of the carbide phases was determined by the Debye-Scherrer type of X-ray patterns. The X-ray patterns obtained from specimens near the boundaries between two types of carbides were generally weak and diffuse as compared with the other patterns. For this reason, and because the more soluble components may be masked, the boundaries between the phases could not be determined precisely. However, the X-ray analysis of electrolytically separated carbides has given consistently reproducible results

Jan 1, 1943

By Walter Crafts, C. M. Offenhauer

In a previous study of the carbide phase of chromium steels, it was shown that chromium carbide (Cr7C3) is 2 more stable carbide than cementite (Fe3C) at tempering temperatures above about 500°C. in quenched steels containing from about I to 7.5 per cent chromium. Below this temperature the carbide phase was found to consist of cementite in all of the steels examined. In the present investigation it was found that a similar change in the carbide phase takes place in molybdenum and in chromium-molybdenum steels at approximately the same tempering temperatures. The approximate ranges of occurrence of the alloy carbides Cr7C3, Cr4C, and Mo2C have been determined in steels containing up to 5 per cent chromium, I per cent molybdenum and 0.60 per cent carbon. The experimental steels were made in small high-frequency furnaces from Armco ingot iron, low-carbon ferrochromium and calcium molybdate and were poured into 2-in. ingots, which were forged to I-in. round bars. Sections of the bars were heated to the carbide-solution temperature and cooled rapidly to induce austenite transformation at relatively low temperatures. The steels were subject to some segregation, therefore comparatively high temperatures were necessary to dissolve all of the carbides. The microstructure of the quenched specimens was examined to verify the belief that the carbides had been dissolved, and also to determine the nature of the nonmartensitic structure of incompletely hardened steels. Ferrite and pseudo-martensite were present in some of the specimens, but all specimens were quenched at such a rate that pearlite was not formed, in order to ensure the formation of the carbides at temperatures lower than about 500°C. It had been found previously1 that in chromium steels the chromium carbide could be produced by transformation of austenite in the pearlite range above 500°C., and, in order to start the tempering treatment with the carbide present as cementite, the absence of pearlite was considered to be essential. The specimens were tempered for 64 hr. to permit the formation of the stable carbide. After tempering, the specimens were submitted to microscopic and X-ray examination. The carbides were separated either electrolytically in a 5 per cent HCl electrolyte or with an acidified copper-potassium chloride solution. The crystal structure of the carbide phases was determined by the Debye-Scherrer type of X-ray patterns. The X-ray patterns obtained from specimens near the boundaries between two types of carbides were generally weak and diffuse as compared with the other patterns. For this reason, and because the more soluble components may be masked, the boundaries between the phases could not be determined precisely. However, the X-ray analysis of electrolytically separated carbides has given consistently reproducible results

Jan 1, 1943

By M. R. Hatfield, F. J. Vosburgh

In a recent article, it was shown that in the blast furnaces in Germany that are lined with carbon blocks no cooling plates are used, and that shower cooling is employed on the hearth and bosh sections. While one of the authors was in Germany he was told that one furnace was being operated without even the shower cooling on the bosh section, though the hearth section was shower-cooled. In discussion of this interesting situation with a number of blast-furnace operators in this country, it was made clearly and promptly evident that shower cooling was very unpopular, probably because of its messiness and its ineffectiveness. Both of the causes for the dislike of shower coolings are reasonable ones. Shower cooling can be and frequently is messy, but the present cooling of blast furnaces leaves much to be desired on that score. Shower cooling is ineffective as compared with plate cooling, so far as its usefulness in keeping the bricks cool enough not to melt or fall to pieces is concerned. However, the introduction of carbon linings changes the situation. No one is concerned with keeping a carbon lining cool, for no temperature in the blast furnace has any effect on carbon, which is just as stable at 3000°F. as it is at 70°F. The only concern is for the shell—to keep it cool enough for safety and comfort— and for that shower cooling is sufficient. Of course, with only the shell to cool, instead of the shell plus all the refractory material, much less water would be required, and the necessity for constant attention to the flow would be lessened, as the hundreds of inlets and outlets would be eliminated. Probably half of the water used in cooling a blast furnace is used for cooling the shaft and tuyeres and the remainder for the bosh and hearth sections. However, in view of the dislike of shower cooling in the United States, and particularly because at least one German blast furnace is operated with no cooling of the bosh section, thought was given to the possibility that a carbon-lined blast furnace might be operated without any cooling of the entire carbon-lined portion. For that reason a series of experiments was performed to determine what might be the temperature of the shell of a blast furnace protected by a carbon lining and operated under varying conditions up to a maximum inside temperature of 3000°F. Experimental Procedure A schematic diagram of the experimental setup is shown in Fig. I and a photograph of the entire assembly in Fig. 2. The heating element was a a tubc nominally 25/8 in. 0.d. by 2 in. i.d. by 30 in., used as a resistor. Power was furnished by a I5-kva. transformer operating

Jan 1, 1942

By M. R. Hatfield, F. J. Vosburgh

In a recent article, it was shown that in the blast furnaces in Germany that are lined with carbon blocks no cooling plates are used, and that shower cooling is employed on the hearth and bosh sections. While one of the authors was in Germany he was told that one furnace was being operated without even the shower cooling on the bosh section, though the hearth section was shower-cooled. In discussion of this interesting situation with a number of blast-furnace operators in this country, it was made clearly and promptly evident that shower cooling was very unpopular, probably because of its messiness and its ineffectiveness. Both of the causes for the dislike of shower coolings are reasonable ones. Shower cooling can be and frequently is messy, but the present cooling of blast furnaces leaves much to be desired on that score. Shower cooling is ineffective as compared with plate cooling, so far as its usefulness in keeping the bricks cool enough not to melt or fall to pieces is concerned. However, the introduction of carbon linings changes the situation. No one is concerned with keeping a carbon lining cool, for no temperature in the blast furnace has any effect on carbon, which is just as stable at 3000°F. as it is at 70°F. The only concern is for the shell—to keep it cool enough for safety and comfort— and for that shower cooling is sufficient. Of course, with only the shell to cool, instead of the shell plus all the refractory material, much less water would be required, and the necessity for constant attention to the flow would be lessened, as the hundreds of inlets and outlets would be eliminated. Probably half of the water used in cooling a blast furnace is used for cooling the shaft and tuyeres and the remainder for the bosh and hearth sections. However, in view of the dislike of shower cooling in the United States, and particularly because at least one German blast furnace is operated with no cooling of the bosh section, thought was given to the possibility that a carbon-lined blast furnace might be operated without any cooling of the entire carbon-lined portion. For that reason a series of experiments was performed to determine what might be the temperature of the shell of a blast furnace protected by a carbon lining and operated under varying conditions up to a maximum inside temperature of 3000°F. Experimental Procedure A schematic diagram of the experimental setup is shown in Fig. I and a photograph of the entire assembly in Fig. 2. The heating element was a a tubc nominally 25/8 in. 0.d. by 2 in. i.d. by 30 in., used as a resistor. Power was furnished by a I5-kva. transformer operating

Jan 1, 1942

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 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, 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 Nathaniel Arbiter, Arthur F. Taggart

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

Discussion of the paper of K. Huessener, (Trans., vol. 53, pp. 402 to 4333, and of the papers of Linn Bradley, H. D. EGbert and W. W. Strong, pp. 303, 319. R. J. WysoR, So. Bethlehem, Pa. (communication to the Secretary*). —At our plant (Bethlehem Steel Co.), we have had several Bradshaw burners under course of construction and erection for some time, but up to the present we have not had opportunity to put them in service. I regret that I can not take part in the discussion with some actual results from these burners. Mr. Huessener properly emphasizes the importance of obtaining the highest combustion temperature practicable in boiler practice, which demands a near approach to perfect combustion conditions. The ideal burner is the one which, while meeting the various mechanical requirements, fulfills the above condition under a wide range of gas pressure. The question as to the relative value of hot raw gas and cold washed gas for boiler use is a very interesting one. I think that in the past the importance of low temperature of washed gas sometimes has been overemphasized. Mr. Huessener has pointed out that so far as temperature is concerned, no advantage accrues in washing gas below 100" F. In many plants, there is a notable operating economy in using furnace cooling water, which is appreciably warmer than the supply water. However, in a given type of washer, other conditions being constant, the lower the exit gas temperature the lower will be the dust content; this is equivalent to saying that the more washing water is used, other conditions being constant, the lower will be the dust content of the exit gas. For each type of washer there is a certain desired average temperature difference between inlet water and exit gas, concomitant with known average dust and moisture contents, and with economical operation. With the present tendency toward smaller stove checkers, it is generally agreed that gas for stove use should be cleaned to a dust content of 0.20 grain or less. The method employed and extent of gas cleaning are clearly problems for individual furnace plants. As a general proposition, wet washing is decidedly more attractive for furnaces smelting soft, fine Lake ores than for those reducing chiefly hard, lumpy ores, such as the foreign and domestic magnetites. In the former case the average moisture content of the gas is probably 35 grains per cubic foot, the dust content is relatively high and the top temperature relatively low. In our plant, the ore mixtures consist almost exclusively of hard magnetites. The average dust content of the gas leaving the dust catcher will average only about 2 grains and the moisture about 12 grains per cubic foot, corresponding to saturation at about 83" F. The temperature is fully 100" F. higher

Jan 1, 1917

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

DISCUSSION I. M. Symonds, (Cia. Minera de Penoles, Monterrey, N. L., Mexico)—Messrs. Boeke and Gunther have written most interesting papers describing their zinc de-leading operations. Mr. Gunther was kind enough to show me his operation last fall. Aside from 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 delead-ing float. The final zinc concentrate still has about 3 pct chalcopyrite, assuming the copper is chalcopyrite, and 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 confined mostly to the conventional lead-zinc 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 handling relatively high grade ores in the mill 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 zinc content we have had to use 0.8 to 1.2 pounds of zinc sulphate per ton of ore with the above cyanide to obtain optimum results. Some time ago we made a laboratory study following Parral and Santa Barbara practice on an ore which had never 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 in the laboratory fresh zinc concentrate from the mill 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 labora-

Jan 1, 1953

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

DISCUSSION I. M. Symonds, (Cia. Minera de Penoles, Monterrey, N. L., Mexico)—Messrs. Boeke and Gunther have written most interesting papers describing their zinc de-leading operations. Mr. Gunther was kind enough to show me his operation last fall. Aside from 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 delead-ing float. The final zinc concentrate still has about 3 pct chalcopyrite, assuming the copper is chalcopyrite, and 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 confined mostly to the conventional lead-zinc 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 handling relatively high grade ores in the mill 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 zinc content we have had to use 0.8 to 1.2 pounds of zinc sulphate per ton of ore with the above cyanide to obtain optimum results. Some time ago we made a laboratory study following Parral and Santa Barbara practice on an ore which had never 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 in the laboratory fresh zinc concentrate from the mill 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 labora-

Jan 1, 1953

By Donald W. Scott

GENERALLY speaking, there is nothing very difficult about taking good micrographs of photogenic thin sections or grains with a petrographic micro-scopecamera setup. However, sometimes it is desired to show some detail that cannot be illustrated satisfactorily by the usual micrographs taken with parallel polarized light, with crossed nicols, or even with two micrographs. A simple procedure giving good results has been used at Battelle Memorial Institute for subjects falling into this classification, and it is believed to be of interest, especially to research people who must sell a point to executives through the medium of well-illustrated reports. The following problem illustrates a typical application: It is desired to photograph a thin section of an iron ore to illustrate the character and association of the iron oxides and the individual quartz crystals. A magnification of 75 dia. is acceptable. A micrograph of the field in question (Fig. I[a]) was taken with parallel polarized light. Due precaution was taken to provide critical illumination, correct exposure, a sharp focus, a good darkroom technique, and other essential conditions. It illustrates correctly the iron oxides, but it fails to show the individual quartz crystals. A micrograph of the identical field (Fig. I[b]) was taken under the same precise conditions, but with crossed nicols. It gives a better idea of the character of the individual quartz crystals but is likely to be misinterpreted unless accompanied by a lengthy descriptive note. This micrograph suggests that the centrally located, large black area is composed entirely of iron oxides. That this is an incorrect interpretation is evident by reexamining the micrograph of Fig. I[a]. The correct interpretation is that the dark area contains quartz crystals oriented with their optical directions parallel to, or nearly parallel to, the vibration directions of the polarizer and analyzer of the microscope. Thus, the executive, or anyone who had not done the work personally, would get no more than a fair interpretation, even if two micrographs were included; and in the interests of both brevity and clarity, one micrograph usually is more desirable. Exactly how many quartz crystals occur in this region cannot be told from the two micrographs, and a printing of the two negatives in register would likewise not show the detail desired. Thus, it is evident that some subjects cannot be satisfactorily illustrated by the usual procedures. In photographing Fig. is the light was subdued and, during the entire exposure of 75 sec., the analyzer nicol was rotated uniformly in its mounting from a crossed position to 45° uncrossed position to introduce the desired amount of contrast in the various individual quartz crystals. The true reproduction of the character and association of the iron oxides, and the additional structure and detail in the quartz areas, is apparent. It might be

Jan 1, 1946

By Edwin T. Myskowski, Alfred H. Hesse

THE development by the U. S. Bureau of Mines of a process for purifying manganese by electrolysis has stimulated interest in manganese alloys. While recent publications have shown some alloys of manganese and copper to possess rather unusual properties, none have included information on tensile properties, which have an important bearing on the usefulness of the alloys. Manganese-copper alloys can be heat-treated, since the single phases that exist at high temperatures may be retained by quenching. According to Persson,1 when quenched alloys containing from about 30 to nearly i00 per cent manganese are reheated, alpha manganese is precipitated (Fig. I). Calculations based on Persson's X-ray data indicate that this decomposi¬tion is accompanied by a change in volume of as much as S per cent. The reason that this large volume change has not been noted probably is the slow rate at which equilibrium is reached by these alloys. In an investigation on hardening by cold-work and heat-treatment, Dean and Anderson3 found that quenched alloys increase in hardness with manganese content and that high-manganese alloys harden very slowly with cold-work, while high-copper alloys harden much more rapidly. Heat-treatment has little effect on manganese-copper alloys containing less than 40 per cent Mn, and affects those alloys containing more than 40 per cent in accordance with their manganese content and heat-treating temperature. Dean and Anderson4 also found that cold-work increased electrical resistance of alloys containing from 50 to 80 per cent Mn, and that heat-treatment of alloys containing from 40 to 96 per cent Mn altered the electrical resistance considerably. Dean, Anderson and Potters have shown that the high vibration damping capacity that characterizes manganese-copper alloys containing 40 to g0 per cent Mn. is affected by cold-work and heat-treatments. Highest vibration damping capacity at low stresses was obtained by heating for 2 hr. at 450°C. (842°F.) after quenching from solution temperatures. Preparation of Alloys.-The alloys for these tests were melted in a 17-lb. basic-lined high-frequency induction furnace using electrolytic manganese, grade A ingot copper and a 70-30 Cu-Mn master alloy (69.80 per cent Cu, 0.12 Fe, 0.04 Si, 0.006 S, 0.07 C, balance Mn). The manganese was heated slowly to expel excess dissolved gases and melted before the addition of copper. No fluxes or covers were used. The melts were cast in tapered iron molds and the ingots were reduced go per cent when forged to ½ in. rounds. These rods were given 2-hr. solution treatments at temperatures that depended upon the composition (Table I). Tensile Tests.-The tensile specimens, 0.313-in. diameter (1.25-in. gauge length), which were enclosed in evacuated Pyrex

Jan 1, 1942

By H. D. Outmans

The author applies the theory of hydrodynamic stability to fluid flow in porous media and concludes that the displacement of miscible liquids is stable if the stability coefficient, as defined by Eq. 19.2 or Eq. 27.0, is positive. The conclusion is invalid, however, since it is based on a faulty argument. To demonstrate this, the reader is referred to Eqs. 4.1 through 4.5 of the paper which describe, in differential form, the first-order disturbances c, u, v, w and p. In these same equations, cx, cz, gl, g3 and are functions of the stable concentration c. This concentration c is known and depends on x, z and t (the author assumes cy = 0). It follows that cx, cz, gl, g3 and µ are also functions of x, z and t. With this in mind, we turn to Eqs. 8.1 through 8.5 which were derived from Eqs. 4.1 through 4.5 by substituting Eq. 6.0. The significance of this substitution is that the author thereby limits the solutions of Eqs. 4.1 through 4.5 to equations of the form of Eq. 6.0. Eqs. 8.1 through 8.5 represent an infinite linear system with five unknowns: c, u, v, w and p. The coefficients cx, cz, gl, g3 and µ in this system are known at each point and at each instant; the coefficients containing derivatives of f are unknown. If this infinite linear system in c, u, v, w and p is to have a nontrivial solution, then it is indeed necessary (as the author states) that the determinant of the coefficient matrix of Eqs. 8.1 through 8.5, i.e., ( A 1, be equal to zero. This condition, however, is not sufficient. A non-trivial solution exists if, and only if, the rank of the coefficient matrix of the entire infinite system is smaller than five. In other words. all minors of order five must vanish and only if all the coefficients in Eqs. 8.1 through 8.5 are constant is this equivalent to the condition |A| =0. Constant coefficients means that gl, g3 and µ, for instance, are constant; and, since they depend on c it follows that c must be constant. We conclude that the condition I A I = 0, on which the author bases his calculations, is necessary and sufficient for a nontrivial solution only if the concentration c is constant. In other words, the author does not investigate the stability of a miscible displacement but, rather, only the stability of the flow of a homogeneous liquid. Using the initial condition and the fact that the coefficients are constant, we find

We the undersigned, being all persons of full age and citizens of the United States and a majority residents of the State of New York, desiring to form a corporation pursuant to the provisions of the Membership Corporations Law for the purpose of incorporating, as provided in Section 5 of Article I. of said law, the existing unincorporated association known as American Institute of Mining and Metallurgical Engineers, Incorporated, do hereby make, acknowledge and file this Certificate for that purpose, and do Certify as follows: I. That the American Institute of Mining Engineers is an unincorporated association organized and existing with the object of promoting the arts and sciences, connected with the economic production of the useful minerals and metals and the welfare of those employed in these industries by means of meetings for social intercourse and the reading and discussion of professional papers, and to circulate by means of publications among its members and associates the information thus obtained. II. That the persons duly appointed or designated to manage the affairs of said association are designated by the rules thereof Members of its Council; that the undersigned are all members of said Council as the same was constituted on the 29th day of December, 1904. III. That on said last-mentioned date a regularly called meeting of said association was held at its office in the Borough of Manhattan, City of New York; that thirty days before such meeting notice of the intention to incorporate said association was given by mail to each member thereof whose residence or post-office address is known; that at said meeting the following resolutions were offered, seconded and duly adopted by the unanimous vote of all its members then present, to wit: "Resolved, That it is the sense of the members and associates of the American Institute of Mining Engineers in general meeting assembled that it is desirable and necessary for the well being of said association and its members and for the furtherance of the objects for which the same has been formed, that said association incorporate under the Membership Corporations Law of the State of New York; "And Further Resolved, That the Members of the Council of this Association, or a majority thereof, be and they hereby are authorized, in accordance with the provisions of Section 5 of Article I. of the Membership Corporations Law, to incorporate this association for the same purposes for which it has been organized and conducted, in the manner provided in Article II. of said law;, "And Further Resolved, That the name of said corporation as hereby adopted by this meeting shall be American Institute of Mining Engineers; "And Further Resolved, That the said incorporators shall be named in the Certifi¬cate of Incorporation as directors of such corporation until its first annual meeting,

Jan 1, 1940

By Jerome J. English, Gordon W. Powell

An experimental investigation and mathematical analysis of the thermal-dilation behavior of the titanium alloy Ti-7Al-3Cb have shown that the linear dimensional changes associated with the polymorphic transformation need not be isotropic. The absolute magnitude of the linear dimensional change, which may be either positiue or negative, associated with the cr-p transformation is dependent upon the relutzve volumes of different orientations of the transformation product. It is hypothesized that the dilation irregulati-ties that have been observed during the polymorphic transformation of pure, coarse-grained titanium and other titanium-base alloys can be explained in the same manner. When titanium is heated above about 165O°F, the hcp a structure transforms to bcc 0. Thermal-dilatioh measurements have shown that the transformation is accompanied by a decrease in length of 0.16 pct.' Such dilation behavior would be expected because the volume of the hcp unit cell is about 0.3 to 0.4 pct greater than that of the bcc unit cell. A recent investigation2 of the thermal-dilation behavior of an experimental a-p* titanium alloy, Ti- 7A1-3Cb, containing 0.06 wt pct 0 showed that its dilation behavior during the polymorphic transformation differed substantially from that reported for unalloyed titanium. The first time the alloy was cycled through the transformation, the dilation curve closely duplicated that of unalloyed titanium. However, upon repeated cycling through the transformation temperature range, both the magnitude and the sign of the dimensional change associated with the transformation were observed to vary with each cycle. This investigation was undertaken to obtain additional data on the dimensional changes associated with the polymorphic transformation in the Ti-7A1-3Cb alloy and to determine the cause of the dimensional irregularities. After testing, the specimens were examined metallo-graphically. In addition, Laue back-reflection patterns were obtained from selected sections taken perpendicular to the specimen axes to determine the a orientations present in these sections. White radiation from a tungsten target and a 0.1-mm-diam collimator were used to produce the diffraction patterns. RESULTS Dilation Curves. Three types of thermal-dilation curves were obtained when the a-8 titanium alloy was heated and cooled through the transformation temperature range. These three types of curves are illustrated in Fig. 1. The type I curve represents what is considered normal behavior, because the dilation change is what would be expected on the basis of the volumes of the unit cells of a and p. The Type I1 curve is the inverse of Type I. Normal behavior is characterized by an expansion on cooling through the transformation, whereas a contraction takes place in the Type 11 curve. With Type ni behavior, no clearly distinguishable length change occurs during the transformation. No other anomalies that might be indicative of other phase transformations were observed in the dilation curves at lower temperatures. Apparently, the cooling rate was low enough for equilibrium to be reached during the 0 to a transformation. Table I lists the types of dilation curves observed during the polymorphic transformation as a function of the direction of measurement and cycle number. The A1 value was determined by extrapolating the low-temperature (a + 5 pct p) and high-temperature (100 pct p) segments of the dilation curves to a common temperature and measuring the difference in the or-dinates at that temperature, see Fig. 1. The transformation occurs over a temperature range in this alloy, so the magnitude of A1 is not an absolute value but depends on the choice of temperature. A mean temperature, T,, within the transformation temperature range was selected for the measurement. T, on cooling occurred about 100°C lower than T, on heating. The first time each of the three dilation specimens was heated to above the temperature, that is, Cycle 2, normal Type I behavior was observed. In Cycle 3, two deviations from normal behavior occurred. First, during cooling of the longitudinal specimen, a substantially larger expansion, +0.21 pct, was measured as 0 transformed to a compared with +0.03 pct in Cycle 2. Second, the thickness specimen was observed to undergo a contraction instead of the anticipated expansion on cooling. Continued cycling of the three specimens from room temperature to 2500°F produced additional changes in the dilation behavior. These changes did not seem to be related to the fabrication direction of the alloy because the values of a1 for the longitudinal, transverse, and thickness specimens varied unpredictably in magnitude and sign. Furthermore, both the longitudinal and transverse specimens showed all three types of dilation curves at least once during the six cycles that they received. Fig. 2 is a sketch of the transverse specimen after

Jan 1, 1967

By V. Leroy, A. G. Guy

Serious disagreements are often found between experimentally determined intrinsic diffusion coefficients and those calculated employing the usual form of the vacancy theory. In the new theory it is proposed that the total intrinsic flux, Ji, of component i, is the sum of a part, f, due to the usual random exclzanges of component i with the vacancies, and a second part, Ji, due to exchanges with the uacancies composing the net vacancy flux. The present treatment, while less powerful than that of Manning, has the advantage of easy uisualization and of facilitating the application of the vacancy-flux effect to complex systems. IT is becoming increasingly evident that there are serious deficiencies in the version of the vacancy theory of diffusion that has been widely used for the past 20 years. One type of evidence is the frequent lack of agreement between intrinsic diffusion coefficients and tracer diffusion coefficients, even taking account of the thermodynamic factor. A second kind of evidence is the observation of a Kirkendall shift larger than theoretically possible, that is, larger than can be accounted for without assigning a negative value to one of the two intrinsic diffusion coefficient.'- The thermodynamic factor could conceivably make both coefficients negative, but not just one. It is clear that a cause of these anomalies, apart from any inadequacy of the usual vacancy theory, might lie in an oversimplified treatment of the data. Adequate experimental techniques, including the use of moderate pressure during the diffusion anneal, are now available to insure that porosity, lateral expansion, and so forth, can be kept negligibly small in most cases. The effect of differences in atomic volume can be of major importance, and it is essential that one of the available methods4 be used to account for this factor. In the present treatment this is accomplished by the consistent use of moles per cubic centimeter as the unit of concentration. Of the various possible inadequacies of the vacancy theory, attention will be given here only to effects of the net vacancy flux. annin' has previously considered this question, beginning with an analysis of atomic jumping of tracer atoms. When he added the effect of a concentration gradient, new terms arose that could be associated with the flow of vacancies. The present treatment uses quite a different approach. The usual vacancy flux, J,, is introduced explicitly, and a simple analysis predicts major changes in the intrinsic diffusion coefficients from this cause. The usual assumptions are made that only a vacancy mechanism is operative, that the formation of voids can be neglected, and that changes in the partial molal volumes, vl and v2, are negligible. The significant diffusion coefficients for the present topic are Dl and D,, the intrinsic coefficients, which enter in the equations, where the flux Ji, moles per sq cm per sec, is that crossing the Kirkendall interface. The concentration, ci, is in units of moles per cu cm, and the concentration gradient, aci/ax, is evaluated at the Kirkendall interface. It will be recalled' that the calculation of Dl and D2 involves the measurement of areas on the diffusion curve with respect to the positions of the Kirkendall and Matano interfaces. In the case of the anomalies mentioned earlier, the Kirkendall shift is too large to be accounted for by the diiferetzce in fluxes (J2 -J1), given by Eqs. [I] and [2]. The logical inference is that the flux of the solvent atoms, J1, is actually in the same direction as the flux of the solute atoms, Jz. In terms of Eq. [I] this requires that Dl have a negative value. However, it would be somewhat misleading to state that the solvent atoms are diffusing up their own concentration gradient. The explanation that will be advanced here pictures competing processes producing the net flux of solvent atoms: 1) diffusion of the solvent atoms down their own gradient by random exchanges with vacancies; and 2) diffusion of solvent atoms in the opposite direction by exchanges with the net vacancy flux. ACTION OF THE NET VACANCY FLUX Theories of vacancy diffusion can be formulated with varying degrees of refinement, and the present theory has purposely been kept as simple as appeared adequate to explain the phenomenon in question. In particular the following aspects have been neglected: 1) the gradient of vacancy concentration in comparison to the gradient of the atomic species; 2) departure of vacancy concentration from the local equilibrium value; 3) variation of the jump frequency, LO, with the specific surroundings of the atom-vacancy pair being considered; 4) correlation effects. These and other refinements can be considered once the essential mechanism has been established. The essential idea of the present analysis is to calculate the total intrinsic flux, Ji, of component i as the sum, JlJ?±j{ [3] where J; is attributable to the usual random atomic jumping, and J{ is a contribution arising from the net vacancy flux, J,. The latter quantity, of course,

Jan 1, 1967

By Martin F. Littmann

Inclusions of MnS and Fe3C have been introduced into single crystals of 3 pct Si-Fe to study their effects on recrystallization behavior and textures after cold rolling and annealing. The presence of MnS in (110) [001] and (111)[112] crystals inhibited primary grain growth and promoted secondary recrystallization but did not alter the texture significantly after annealing at 1200°C. The presence of Fe3C in (llO)[OOl] and (100)[001] crystals caused a refinement of the primary re crystallized grain size but did not promote secondary recrystallization. THE texture behavior of single crystals of 3 pct Si-Fe during deformation and recrystallization has been studied by numerous investigators. The early work of Dunn&apos; followed by Decker and Harker2 involved relatively small cold reductions. More detailed studies of Dunn3&apos;4 and of Dunn and Koh5&apos;6 involved a reduction of 70 pct and recrystallization at 980°C for several crystals. Walter and Hibbard7 studied a greater variety of initial orientations and sought to relate the textures to those of polycrystalline material. Attention was focused on the nucleation process during early stages of annealing and on surface energy effects in studies by Walter and Dunn8 and by HU.9&apos;10 One of the most extensive investigations has been reported by T. Taoka, E. Furubayashi, and S. Takeuchi.11 Most of this work has been conducted using relatively pure crystals with minimal amounts of precipi-tate-forming elements such as carbon, oxygen, sulfur, and nitrogen. Recently, however, S. Taguchi and A. Sakakura have observed that AIN precipitates can alter the recrystallization textures of rolled (100)[001] crystals.12 The present studies were initiated to determine effects of MnS and Fe3C precipitates on recrystalli-zation and grain growth behavior of rolled single-crystals of 3 pct Si-Fe. Both of these types of inclusions play significant roles in the recrystallization behavior leading to the formation of the (110)[001] or cube-on-edge texture in commercial grain-oriented silicon iron. It is well known that (110)[001] primary grains are formed by recrystallization of (110)[001] or (11 l)[ 112] crystals after cold reduction of about 60 pct or more. Crystals of these orientations, therefore, were selected for study of the effect of MnS in-clusions on grain growth. On the other hand, a major component of the texture of cold-rolled, polycrystal-line 3 pct Si-Fe is the (100)[011] orientation. The function of Fe3,C inclusions is of interest for this orientation. EXPERIMENTAL PROCEDURE The single crystals used are listed in Table I and were obtained from commercial Si-Fe alloy processed to produce (110)[001] and (100)[001] texture by secondary growth. The cube-on-edge material was 0.59 mm thick. Suitably large (110)[001] crystals 25 mm wide were selected and their orientations were determined using an optical goniometer. Etch pits for texture determination were formed by a ferric sulfate solution. The other crystals used in the study with (100)[001], (100)[011], and (111)[112] orientations were obtained from sheet which contained large grains developed from secondary recrystallization by a surface-energy driving force.13 Most crystals had a (100) plane very nearly parallel to the sheet surface and the rolling direction could be selected readily. The same sheet also contained a few crystals with (111) planes parallel to the sheet surface, these also being a result of growth by surface energy. The crystals selected from the sheet were about 25 mm wide and 0.25 to 0.28 mm thick. As shown in Table 11, the crystals already contained about 0.070 to 0.10 pct Mn. Inclusions of MnS were incorporated into crystal 36 in the following manner. The crystals were first sulfurized by holding them Table I. Initial Orientations of Crystals Crystal No. Initial Orientation Thickness, mm Special Treatment 34 (I10) [00l]* 0.59 None 36s (110) [001] 0.59 Sulfide precipitates added 30,40 (111)[Ti21 0.28 None 43s (III) [Ti21 0.28 Sulfide precipitates added 37 (100) [Oll] 0.30 None 37C (100) [01I] 0.27 Carbon added 41 (100) (01I] 0.25 None 41C (100) [OI11 025 Carbide precipitates added 42 (100) [OOl] 0.25 None 42C (100) [001] 0.25 Carbide precipitates added *Tilted 4 deg to r~ght about R.D. Table II. Compositions of Crystals Special Treatments Base Analysis ~ ______________________£________________Crys- Crystals Pct Si Pct C Pct Mn Pct S Pct N Pct Al tal Pct C Pct S 34.36 2.93 • 0.099 <0.005 - 0.0014 36S 0.011 30.37 to 42 2.78 0.0057 0.070 0.001 0.0008 0.0011 43S 0.022 37C 0.029 -41C 0.028 -42C 0.026 *Estimate 0.004 pct. Oxygen estimated <0.003 pct on all samples

Jan 1, 1970

By F. B. Harris

MINE surveying and engineering at the various properties of the United States Smelting Refining and Mining Company has developed and increased in importance steadily as mining methods have changed and expanded, both in the development of ore bodies and in the methods and styles of stoping. Most important to satisfactory engineering practice, and secondary -only to accuracy and precision, is the preservation of all data relative to surveys and calculations so that it is readily available for use at all times and in -such form that it is permanent, easily found, and usable. The first consideration for a proper, accurate, and practical start for surveys and efficient engineering at any property is an accurate triangulation net and system of co-ordinates. This has been our practice and the first step seas to select a base line, readily accessible and easily measured, situated preferably on an even grade where the difference of elevation between the two -end monuments was not too great and -the distance was long enough for practical use. Permanent concrete monuments were built for these base-line points so constructed that they could be easily recognized and were visible. Precise levels were run on this base &apos;line and the elevation (sea level datum) if possible was established at each end monument. The distance was carefully measured many times, back and forward, by using a tape that had been standardized by the National Bureau of Standards. The tape was supported at ,each 25-ft interval on stakes which had been brought to grade between each measuring point. All conditions were

Jan 1, 1948

By Fred D. Fox

INTRODUCTION Approximately two years have elapsed since the first summary of the Grizzly Gulch Tailings Disposal Project was presented (1). Since that time, various physical modifications and additions to the existing treatment system have transpired. Further, Homestake and the entire mining industry have been impacted severely by additional modifications and additions concerning regulatory reform aimed at total disciplinary permitting and hazardous waste management. The following paper summarizes the past accomplishments relating to the Grizzly Gulch Tailings Disposal Project, correlating these accomplishments with future plans that are being developed to comply with regulations and to continue Homestake&apos;s commitment to environmental protection. The famous Homestake Gold Mine, located in Lead, South Dakota, has been operating in the Black Hills region for over a century, approximately 12 years before the south half of Dakota Territory was admitted to the Union as the State of South Dakota (2). During the 104 years of operational development, Homestake&apos;s Gold Mine, as well as the entire mining industry, have been influenced by numerous governmental regulations dating back to the Refuse Act of 1899 which regulated the deposit of debris from mines and stamp works. The enactment of the National Environmental Policy Act of 1969 may be thought of as the beginning of a long line of unplanned steps to deal with the many concerns of matters pertaining to the environment. Environmental awareness continued into the 1970’s, in which the Clean Air Act, Federal Water Pollution Control Act, Safe Drinking Water Act, Toxic Substances Control Act, and the Resource Conservation and Recovery Act (RCRA), to name a few, surfaced.

Jan 1, 1983