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By William J. Robinson

What is the cumulative rate of recovery of copper from a sulfide leach dump? The technical answers to this frequently asked question may vary from "I don't know" to "quite good" from people of the same company. Management also poses this question because it plays a vital role in planning future production. The answer is difficult because of the many variables between different operations such as physical construction of the dump, topography of the original site, characteristics of dump material, mineralization, and water application. Each of these factors and others have a bearing on the rate of recovery. Anaconda's method of water distribution at Butte is unique in that each dump is drilled to allow physical injection of water into the dump. The injection holes are drilled vertically on 25-ft centers from the surface of the dump [(Figs. 1 and 2)]. Normally, the holes are drilled 40 ft deep and cased with 4-in. PVC perforated pipe. The pipe is perforated at 1-ft intervals with four 1 -in.-diam holes at 90° spacing on the pipe circumference. Formerly, shallow holes (20-40 ft) were alternated with deep holes (80-180 ft) in an effort to cover the entire dump and hasten oxidation. The shallow hole depth varied according to the compaction thickness. The deep hole depth varied according to the height of the dump and the original ground profile. It is preferable to have the deep holes end 20-30 ft above the original ground level. This generally allows penetration of the coarse material at the bottom of the dump. Deep holes had to be discontinued in order to cover more

Jan 1, 1974

By W. J. C. Venter

The use of activated carbon to improve the selectivity in the separation of base metal minerals from bulk concentrates played an important role in the development of separation techniques employed at Tsumeb and Kombat mines. The Kombat mine, owned and operated by Tsumeb Corp. Ltd., is located in the Otavi Valley in the northern part of South West Africa, approximately 213 air miles north of Windhoek and 38 air miles south of Tsumeb, at latitude 19° 43'S and longitude 17º 41'E. The mine is linked to all major centers by both national railroad and tarmac highway systems which pass right through the town. The Otavi Minen- and Eisenbahn-Gesellschaft (OMEG) mined ore on the farm Asis from 1908-1925. Tsumeb Corp. Ltd. acquired the mineral rights in 1947, started diamond drilling in 1954 and commenced mine development in 1960. The mill started production in 1962 when proven ore reserves were 3,378,084 st containing 2.85% Cu and 2.90%Pb. Annual production of 248,411 st was increased in May, 1967 to the rate of 422,990 st, which was still being maintained in 1971, when ore reserves stood at 3,054,701 st of grade 1,91% Cu and 2.5% Pb.

Jan 4, 1973

By T. G. Sieber, T. D. Tiemann

The extraction of quartz from siliceous iron ores by dissolution in sodium hydroxide solution has been described in detail in AIME Transactions. l923 data reported covered the temperature range from 230-416°F, where a continuous increase in the amount of silica extracted with increase in temperature was found. It is the purpose of this paper to describe some unexpected results of more recent work exploring principally the range of 500600°F where higher rates and greater amounts of silica extraction were antici-p ted. In brief, the experimental procedure consists in digesting the ore under pressure in solutions of sodium hydroxide, filtering the suspension and weighing and analyzing the dried residue for iron content. The amount of extraction is calculated from the weight loss or from the iron analysis of the residue and that of the original ore.

Jan 1, 1969

By Albert Zima

ACCORDING to recently published statistics, it is predicted that as much oil must be produced during the next 16 years as has been produced during the past 75, in order to satisfy the high rate of consumption of petroleum products. During 1934, over 17,000 oil wells were completed in the United States, and it is expected that over 20,000 additional wells will be drilled during the current year. Were it not for the remarkable progress made during recent years in the improvement of drilling technique and in the development of equipment used in the production phase of the oil industry, it is doubtful whether sufficient oil could be produced to meet present requirements. A few years ago, wells seldom were deeper than 3500 to 4000 ft., owing to the limitations of the drilling methods and equipment employed. Today, however, through the application of scientific drilling methods and the adaptation of modern equipment and improved materials, many wells range from 6000 to 8000 ft. in depth, and a few recent completions exceed 10,000 feet.

Jan 1, 1935

By Charles Legrand

(San Francisco Meeting, September, 1915) THE problem of mine pumping is so much affected by local conditions, and those conditions are so liable to changes during the life of a mine, that the best system to use is difficult to determine. The experience of the;, writer has been that, in general, for copper mines, electric pumping is most satisfactory unless the quantity of water to be pumped is great or. the mine does not use electric power for any other purpose. As a rule, however, figuring on the cost of necessary power plant, the total cost of: installation is greater with electric pumps than steam- pumps. As the water is liable to be gritty, outside-packed plunger pumps are to be recommended, and if the water is not acid, or only slightly so, chilled cast-iron plungers pay for their extra cost very quickly in diminished cost of packing. With chilled plungers it is possible to use metallic, packing instead of soft packing, if the water, is not too gritty nor the lift too high. In vertical pumps this packing is satisfactory for lifts up to 400 ft., in the experience of the writer; and may be found satisfactory for higher lifts. For water slightly acid, cement-lined pump bodies have given good satisfaction. For acid. water, both plungers and pump bodies should be made of acid-resisting bronze. For high lifts, especially with gritty water, a satisfactory pump valve is difficult to find. To reduce the unbalanced pressure on the valve at time of opening it is advisable to have narrow seats; this, however, brings high pressure on the seats when the valve is closed. On large valves for lifts of 600 to 1,000 ft. we have used leather, hard rubber, vulcanized fiber, and soft brass; for clear water the latter has given best satisfaction. The difficulties due to grit make it advisable to have large sumps where water can settle, and if possible, to have two of them so that they can be cleaned alternately. At the mines of the Old. Dominion Copper Mining ,& Smelting Co.; Globe, it was found that a small air. ejector discharging into a mine car is a very convenient way to clean mud and sand from a sump. .

Jan 9, 1915

By P. D. White, J. T. Moss, J. S. McNiel

Results of experimental work on the in situ combustion process were first published in this country in 1953' when Kuhn and Koch described results of a three-well test in Jefferson County, Okla. Shortly there-after Grant and Szasz2 described field studies in Nowata County, Okla., in which several modifications of the basic combustion process were investigated by injection of various oxidizing gas mixtures other than air. In the past five years speculation concerning this method of oil recovery has continued, with a number of interesting papers on various aspects of in situ combustion appearing in the literature3,4,5,6,7. However, only one of these' provided actual engineering information on pattern-type field experiments. The primary objectives of the Oklahoma three-well test were to check operation of specially designed electrical ignition equipment and evaluate problems associated with initiation of combustion in a natural oil sand reservoir. Immediately following successful completion of this test in the Pontotoc sand, plans were activated for a second field experiment to be conducted in the same sand a short distance away. The objective of this second field test1 as to establish a relationship between field observations and information derived from laboratory experimentation and computations. Secondary objectives of the test were to develop operating tech- niques and define operating problems, and to obtain information that would assist in the economic and engineering appraisals of the process. Careful planning was required since this test was designed with the hope of providing basic information on the characteristics and operation of a combustion drive. It was necessary to include test facilities which would not only permit precise control and measurement of the process variables but would also provide sufficient flexibility of control to insure that variables in the combustion process could be studied during the course of the test under a wide range of conditions. In order to accomplish these objectives elaborate instrumentation and several control wells were included in the design of the test installation. This type installation was felt to be well suited for an experimental study, but was in no respect intended as a counterpart of a commercial-scale operation. PRELIMINARY LABORATORY WORK An important objective of the field experiment, as stated previously, has been to obtain reliable data on operating variables which might be compared with similar data obtained in laboratory combustion tests. The value of successful correlations between quantities that can be measured in the laboratory and those obtained in a full-scale commercial venture has been well established for other industrial processes. The difficulty of following a process underground should make such correlations even more essential here. Also. approaching the field test phase of development of in situ combustion, it was considered desirable to precede design of test equipment with laboratory combustion studies under a variety of conditions to establish likely ranges of variables. These included temperature, air injection rate, frontal advance rate and produced gas composition.

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

THe elements silver, cadmium, tin, antimony and tellurium either are found as impurities in commercial coppers or are intentionally added to produce coppers for special uses. When present in small quantities, each of these metals exerts a significant effect on the properties of copper, but despite considerable experience and investigation much remains to be learned about their specific behavior. The presence of extraneous elements, particularly oxygen, complicates the study of individual additions of impurities in the range o to 0.05 per cent, and the use of high-purity copper has been found extremely helpful in circumventing these difficulties. It has also been found that individual behavior can be satisfactorilv determined from measurements of two commercially important properties, conductivity and softening temperature, according to methods that have been described previously.1,2 Data of this type, obtained in the course of a general investigation of the effects of impurities on the properties of both oxygen-bearing 2nd oxygen-free copper are presented herewith. All samples except those containing cadmium were prepared as 3/8-in. continuously cast oxygen-free rod from pure copper and weighed amounts of a similarly synthesized master alloy. Composition was checked by chemical methods, which in every case verified the calculated analyses. Test wires were cold-drawn one B, and S. number per pass on a string-up machine using four 30-min. 600°C. anneals at 0.3125, 0.257, 0.204 and 0.162 in. and a final cold reduction of 75 per cent to 0.081 in. Some oxygen-bearing samples were produced directly from the 3/8-in. oxygen-free rods by diffusion from a surface scale at 850°C. and drawn to size as listed above, but most of the alloys were remelted in pure graphite and cast through air into a I-in. round mold. The slugs were then hot-rolled to 5/16 in., drawn to 0.162 in., annealed as listed above, and drawn to 0.081 inch. Conductivity wires were annealed for I hr. at 100°C. intervals between 300' and 800°F., using a hydrogen atmosphere for oxygen-free samples and purified nitrogen for the oxygen-bearing type. All samples were quenched from the annealing temperature in 10 per cent H²S04 and conductivity was measured on a Hoopes bridge that had been checked against a Kelvin bridge. The softening temperatures represent the half-hard stage of the annealing curve as determined by a standard procedure.' Effect of Silver Numerous excellent studies of the argentiferous coppers are found in the literature, and these have been adequately

Jan 1, 1943

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

THe elements silver, cadmium, tin, antimony and tellurium either are found as impurities in commercial coppers or are intentionally added to produce coppers for special uses. When present in small quantities, each of these metals exerts a significant effect on the properties of copper, but despite considerable experience and investigation much remains to be learned about their specific behavior. The presence of extraneous elements, particularly oxygen, complicates the study of individual additions of impurities in the range o to 0.05 per cent, and the use of high-purity copper has been found extremely helpful in circumventing these difficulties. It has also been found that individual behavior can be satisfactorilv determined from measurements of two commercially important properties, conductivity and softening temperature, according to methods that have been described previously.1,2 Data of this type, obtained in the course of a general investigation of the effects of impurities on the properties of both oxygen-bearing 2nd oxygen-free copper are presented herewith. All samples except those containing cadmium were prepared as 3/8-in. continuously cast oxygen-free rod from pure copper and weighed amounts of a similarly synthesized master alloy. Composition was checked by chemical methods, which in every case verified the calculated analyses. Test wires were cold-drawn one B, and S. number per pass on a string-up machine using four 30-min. 600°C. anneals at 0.3125, 0.257, 0.204 and 0.162 in. and a final cold reduction of 75 per cent to 0.081 in. Some oxygen-bearing samples were produced directly from the 3/8-in. oxygen-free rods by diffusion from a surface scale at 850°C. and drawn to size as listed above, but most of the alloys were remelted in pure graphite and cast through air into a I-in. round mold. The slugs were then hot-rolled to 5/16 in., drawn to 0.162 in., annealed as listed above, and drawn to 0.081 inch. Conductivity wires were annealed for I hr. at 100°C. intervals between 300' and 800°F., using a hydrogen atmosphere for oxygen-free samples and purified nitrogen for the oxygen-bearing type. All samples were quenched from the annealing temperature in 10 per cent H²S04 and conductivity was measured on a Hoopes bridge that had been checked against a Kelvin bridge. The softening temperatures represent the half-hard stage of the annealing curve as determined by a standard procedure.' Effect of Silver Numerous excellent studies of the argentiferous coppers are found in the literature, and these have been adequately

Jan 1, 1943

By Reamy Joyce

CONDITIONS in underground mining are so variable that in approach-ing the problem of the economies effected by the use of pressure-treated mine ties and mine timbers, it is necessary to secure specific data for each mine. Facts must first be dug out to show the service life of untreated timber and the reason for its failure. Generally speaking, decay is the usual cause of failure, but in some mines mechanical destruction is an important factor. Occasionally the two causes combine to produce fail-ures, and it is difficult to determine positively which factor is responsible. In making comparisons, it is always necessary to start with the cost in place and for this reason there must be accurate information covering the labor cost of installation and the labor cost of renewals. When treated timber is used, it is necessary to know the specifications for the treating process, whether the timber was painted, dipped, treated open tank, or impregnated under pressure according to standard specifica-tions. It is also necessary to know the preservative used and the amount of the preservative that was retained by the timber after treatment. It is also well to know whether the timber was thoroughly air-seasoned before treatment or was green at the time it was treated. The kind of timber available, both untreated and treated, must be known and all of the factors listed above must be taken into consideration in the study of any problem.

Jan 1, 1939

(Members are urged to send in for this column any notes of interest concerning themselves or their fellow-members) Members and guests who called at Institute headquarters during the period Jan. 10, 1917 to Feb. 10, 1917: Victor C. Alderson, Denver, Colo. G. Komar, New York, N. Y. Arthur W. Allen, New York, N. Y . H. H. Lauer, Allentown, Pa. George S. Blair, Pittsburgh, Pa. Frederick MacCoy, Antofagasta, Chile. F. J. Brulé, Toronto, Canada. E. P. Mathewson, Toronto, Canada. W. M. Corse, Buffalo, N. Y. Douglas Muir, San Antonio, Tex. John J Croston, Cullasaja, N.' C. F. W. Osborn, Ajo, Ariz. W. A. Deane, Waxhaw, N. C. Mortimer A. Sears, Washington, D. C. P. H. Dudley, New York N. Y. W. H. Selden, Jr., Iron River, Mich. J. D. Gilchrist, Denver, Colo. W. H. Staver, Yonkers, N. Y. L. Hoffman, Pottersville, N. J. Ralph H. Sweetser, Easton, Pa. Guy R. Johnson, Florence, Wis. Benjamin F. Tibby, Salt Lake City, Utah. W. McA. Johnson, Hartford, Conn. Carl J. Trauerman, Butte, Mont. John S. Kennedy, Philadelphia, Pa. H. C. Wilmot, Arequipa, Peru. D. C. Bard has become a member of the geological department of the Chicago, Milwaukee & St. Paul R. R., with headquarters at Seattle. Jay A. Carpenter has resigned his position as metallurgist for the West End Consolidated at Tonopah and has been appointed superintendent of flip. Nevada. Packard mines it Rochester.

Jan 3, 1917

By Francis M. Walters

THE problem of making iron-manganese alloys of scientific purity is a rather difficult one. They cannot be prepared in air because of the readiness with which the metals oxidize at the temperature of melting; and they cannot be prepared in vacuum because of the, high vapor pressure-of- manganese. The very property of: manganese which permits it to be purified interferes with the utilization of the best method of making pure alloys. Accordingly, it is necessary to use a gas atmosphere which will not affect the-properties of the alloys. The gases available for the purposes are hydrogen; helium and argon. Nitrogen forms intermetallic compounds with manganese very readily. Hydrogen, while valuable as a deoxidizer and having the advantage of being comparatively cheap, is explosive over a wide range and, has a rather high thermal conductivity. Helium is reported as, costing little but is difficult to secure at a reasonable price and also has a conductivity nearly as high as hydrogen. Since argon has a sufficiently low thermal conductivity, it has been selected for use in one induction furnace for melting, under a controlled, gas atmosphere, in spite of its cost, which is so high (70 cents to $1.50 per cubic foot) that it must be stored and purified.. Such a gas atmosphere-as argon makes necessary the use of the, high-frequency induction method of heating. This involves, a non-metallic container for the gas; .which is most conveniently of fused quartz or glass. The next

Jan 1, 1929

By L. Stone, H. Margolin

The Ti-C-N and Ti-C-O systems were investigated in the temperature range from 500° to 1400°C and in the composition range up to 2 pct C and 5 pct N or 0. Characteristic isothermal sections at 800°, 900°, 1000°, and 1300°C are presented. The Ti-N-0 system was studied in the temperature range from 900' to 1400°C with alloys containing up to 6 pct total alloying content. Characteristic isothermal sections at 1000° and 140O°C are presented. Melting-point data for all three systems are also included. THIS paper reports on one of a series of investi-gations which have been conducted on the phase diagrams resulting from interstitial alloying with iodide titanium. The other investigations involved delineation of the binary systems with carbon,' nitrogen and boron,h and oxygen. The Ti-0 binary system has also been investigated by Bumps et al.' In varying degrees, each of these interstitial elements has been shown to stabilize the low temperature a modification of titanium1-5 and each forms a face-centered cubic TiX compound (henceforth designated 6). In addition, the Ti-N and Ti-0 systems reveal a low temperature tetragonal phase (6) formed by a peritectoid reaction between a and TiX Experimental Procedure The development of experimental techniques for the study of titanium alloy systems has, to a large extent, become standardized. In this investigation, the equipment and procedures described in detail by Cadoff and Nielsenl have been used. Arc Melting: In general, binary alloys with carbon, nitrogen, and oxygen, prepared in the composition range of interest in this investigation, show negligible composition changes during arc melting. However, the possibility of the formation of some gaseous combination of alloying elements such as CO, CN, or NO during the preparation of these ternary alloys was considered. Calculations showed that the evolution of only 0.05 gram of such a gas would be detectable as a pressure change in the closed system used during preparation of these alloys. Such pressure changes were not observed. Consequently, nominal compositions have been used in plotting the data. The compositions of the materials used in the preparation of the alloys are shown in Table I. After melting for 3 to 5 min at 275 to 350 amp, the alloys were checked for homogeneity by microstruc-tural examination. Alloys containing up to 1 pct C were homogeneous in the presence of less than 3 pct N or 0. At higher alloying contents, some inhomo-geneities in the carbon distribution became evident. Alteration of the melting procedure toward longer times and higher currents did not improve the homogeneity of these alloys. Ti-N-0 alloys were homogeneous in the range to about 3 or 4 pct total alloying addition. Beyond this, almost all of the specimens showed as-cast microstructures consisting only of the phase. Consequently, inhomogene-ities could not be detected by examination of micro-structures. Ten alloys from each of the systems were analyzed for two of the elements present (oxygen being omitted in all cases and titanium being omitted in the Ti-C-N alloys). In all cases the analyses were found not to be sufficiently precise to serve as criteria for the total composition of these alloys. On the basis of phase distribution in heat-treated alloys, however, it appears that carbon is distributed throughout the alloys most uniformly, with oxygen and nitrogen following in that order. Heat Treatment: Specimens for heat treatment were wrapped in titanium sheet before sealing in the argon-filled quartz capsules. Heat-treatment times varied from 100 hr at 800°C to 0.5 hr at 1400 °C. After heat treatment the specimens were quenched by breaking the capsule in water. With the exception of alloys in the low composition region, heat treatment did not have an appreciable effect on the as-cast microstructures. Metallography: Following heat treatment, the specimens were prepared for metallographic examination by grinding on emery paper and electrolytic polishing. For the majority of the specimens a 10-sec etch with Remington "A" agent (25 pct HNO3, 25 pct Hf, and 50 pct glycerin) adequately

Jan 1, 1954

By M. E. Wadsworth, T. D. Chatwin

The kinetics of sulfidization of hematite (Fe203) by H2S gas at various partial pressures have been determined over the temperature range of 170° to 500°C. The process was controlled by thin films of pyrite (FeS2) and troilite (FeS) which were protective and formed diffusional layers. At higher temperatures the thermodynamic drive to form FeS2 decreased, and consequently the rate of formation of FeS, decreased. Conditions for the development of thin layers of FeSz consisting of 10 to 100 atomic diameters are presented. Laboratory flotation results on synethetic ores indicate floatability identical to that of pyrite of normal xanthate flotation. The prospect of high-temperature sulfidization of metal oxides using H2S, S, or other sulfur bearing compounds is intriguing as a potential activation process for flotation since the thermodynamics are very favorable for a large number of systems. If the kinetic parameters are sufficiently well understood it may be possible to provide surface sulfide layers a few angstroms thick, thus imparting normal sulfide floatability characteristics to the oxide. For thin layers the total sulfur pick-up would be small except for very high surface area materials but in most cases this sulfur could be readily removed by roasting if necessary. The general reactions for the sul-fidization of metal oxide MxO, to a metal sulfide MpSq using H2S may be written for the three conditions py > xq; py < xq; and py = xq: A large thermodynamic advantage is obtained in many systems because of the relatively large negative free energy of formation of H,O compared to H,S. For the temperature range 2S° to 1500°C &apos; where AFOis the standard free energy and T is absolute temperature. As is evident from Eqs. 4 and 5, the free energy of formation of H ,0 is approximately 35 to 37 kilocalories per mole greater than that for H,S over broad variations of temperature. For oxide-sulfide systems as outlined above, sulfidization may be expected to occur for the conditions: Groups I and 111: that is, if the terms on the right are more negative than those on the left the reaction is expected to occur thermodynamically. The value hFg,(,) is included in Eq. 6 since hFLzs is based upon gaseous S2 rather than the normal reference state, orthorhombic sulfur. The

Jan 1, 1969

By John T. Norton

N order to attempt to arrive at a better under-Jl standing of the whole basic problem of sintering, these remarks will serve as an introduction for discussion that is included and will, perhaps, help to isolate specific questions which need to be answered or to suggest some definite avenues of investigation which should be followed. To bring some sort of logical order into the presentation, I will consider the various types of interaction between the metal to be sintered and the atmosphere which surrounds it, depending upon whether the phenomena are essentially chemical or physical in nature. For example, when the only necessary criterion for the satisfactory sintering of a certain powder is the removal of an oxide skin, then the problem of choosing a suitable atmosphere is primarily chemical; however, if a special surface condition as a consequence of the oxide skin removal is necessary for particularly effective sintering, then the problem becomes a physical one. Of course, the two aspects overlap considerably, but it may be possible to make a distinction in principle if not in practice. The chemical characteristics of the phenomena will be emphasized, since these are the better known. Metal-gas reactions involved in sintering are controlled primarily by the thermodynamics of the processes involved. In which direction will a reaction go and how far before it stops? The answer is to be found in the magnitude of the free energy change associated with the reaction. If a constituent is to be removed from the specimen as completely as possible or if a constituent is to be formed in the specimen as completely as possible, then one chooses conditions which are far from equilibrium so that the reaction is driven toward completion. On the other hand, if the composition is to be maintained at a desired value, then conditions are adjusted as closely as possible to the equilibrium point. This aspect of the problem is susceptible to quite precise analysis, provided, of course, that the significant reactions can be recognized and the required thermodynamic data are available. Conversely, if one asks how fast the reaction goes or how far it proceeds in a given time, the answer is frequently much more difficult to answer in quantitative terms. Yet the rate-con trolling factors of the reactions may be of primary importance in the success of a particular operation, especially where competing processes are at work. Both equilibrium and rate factors must be understood if a clear picture is to be obtained. For instance, in a process for carburizing titanium dioxide, is the difficulty of obtaining a stoichiometric Tic due to a true limitation of the equilibrium or simply to a very slow rate of reaction? An example of this appears in the work of Kalish and Mazza.&apos; They showed that the oxygen content of sintered iron compacts was lower when sintered in pure hydrogen than in the case where the hydrogen was diluted with either argon or nitrogen. The equilibrium oxygen content of the iron would be the same in the two cases, since it is determined by the ratio of the partial pressures of water vapor and hydrogen and this pressure ratio is unchanged by dilution. The rate of oxygen removal, however, under the conditions of a constantly replaced furnace atmosphere, depends upon diffusion and thus upon the concentration of hydrogen in the furnace atmosphere. Possibly the clearest way to illustrate the interplay of these two factors is to consider in more detail some of the typical metal-gas reactions. Adsorbed Gases It is common experience that fine metal powders with their very large surface areas often contain large quantities of gas. This gas, which results from exposure to air or perhaps from some step in the

Jan 1, 1957

By Earnshaw Cook, H. S. Avery, J. A. Fellows

TEe increased use of heat-resistant alloys (26 per cent Cr, 12 per cent Ni; 16 per cent Cr, 35 per cent Ni; 12 per cent Cr, 60 per cent Ni; etc.) in recent years has been accompanied by continued demands by the consumer for improvement in properties. The manufacturers of these materials, of necessity, have resorted to more critical studies of the basic causes of variations in fundamental properties. To keep pace with the need for augmented information, previous techniques of investigation have been refined and new test methods and instruments created. It is the purpose of this paper to describe the apparatus, experimental technique and precision of measurement that were employed in the exploration of properties of heat-resistant alloys presented in a companion paper. The detailed precautions in experimental procedure essential for attainment of accurate and comparable data at elevated temperatures cannot be too highly emphasized. The Creep Test Since the fundamental concepts of creep testing have been recognized for the past 20 years, present interest is restricted to refinements in equipment and experimental procedure. The creep-test iaboratory constructed for the American Brake Shoe and Foundry Co. is designed to permit I000-hr. tests in the temperature range of I200° to 2 200°F. with a choice of applied stress extending from jo to 50,000 lb. per sq. in. in increments of 50 lb. per sq. in. To simplify the calculation of weight combinations, the loading beams (Fig. I) are provided with counterweights to eliminate the tare. The precision of the knife-edges (10:I ratio) is such that a 10-gram weight placed on the upper specimen grip will be exactly balanced by a I-gram weight attached to the loading shackle. Check of the loading weights proved the maximum error to be 0.06 per cent. Axial alignment is provided by crossed knife-edges in the grip seats. The furnaces are similar in design to those of Crane and Company, Battelle Memorial Institute, and the U.S. Steel Corporation. An 80 per cent Pt, zo per cent Rh No. 19 B. and S. gauge wire is used as the heating element. The details of -construction are shown in the radiograph reproduced in Fig. 2. The windings are held in place on an alundum tube with aludum cement; the distribution of turns is adjusted to give a maximum temperature gradient of , I°F. over a 4-in. gauge length (Fig. 3). To avoid sharp temperature differentials at the ends of the test section, the length of the furnace is four times the gauge length. Sixteen-inch coupons are used „ to reduce the temperature of the threaded joints and thus to facilitate removal from the grips. Thermal losses are minimized by refractory insulators cut to shape and surrounded by diatomaceous ear,th. The taps

Jan 1, 1942

By J. A. Fellows, Earnshaw Cook, H. S. Avery

TEe increased use of heat-resistant alloys (26 per cent Cr, 12 per cent Ni; 16 per cent Cr, 35 per cent Ni; 12 per cent Cr, 60 per cent Ni; etc.) in recent years has been accompanied by continued demands by the consumer for improvement in properties. The manufacturers of these materials, of necessity, have resorted to more critical studies of the basic causes of variations in fundamental properties. To keep pace with the need for augmented information, previous techniques of investigation have been refined and new test methods and instruments created. It is the purpose of this paper to describe the apparatus, experimental technique and precision of measurement that were employed in the exploration of properties of heat-resistant alloys presented in a companion paper. The detailed precautions in experimental procedure essential for attainment of accurate and comparable data at elevated temperatures cannot be too highly emphasized. The Creep Test Since the fundamental concepts of creep testing have been recognized for the past 20 years, present interest is restricted to refinements in equipment and experimental procedure. The creep-test iaboratory constructed for the American Brake Shoe and Foundry Co. is designed to permit I000-hr. tests in the temperature range of I200° to 2 200°F. with a choice of applied stress extending from jo to 50,000 lb. per sq. in. in increments of 50 lb. per sq. in. To simplify the calculation of weight combinations, the loading beams (Fig. I) are provided with counterweights to eliminate the tare. The precision of the knife-edges (10:I ratio) is such that a 10-gram weight placed on the upper specimen grip will be exactly balanced by a I-gram weight attached to the loading shackle. Check of the loading weights proved the maximum error to be 0.06 per cent. Axial alignment is provided by crossed knife-edges in the grip seats. The furnaces are similar in design to those of Crane and Company, Battelle Memorial Institute, and the U.S. Steel Corporation. An 80 per cent Pt, zo per cent Rh No. 19 B. and S. gauge wire is used as the heating element. The details of -construction are shown in the radiograph reproduced in Fig. 2. The windings are held in place on an alundum tube with aludum cement; the distribution of turns is adjusted to give a maximum temperature gradient of , I°F. over a 4-in. gauge length (Fig. 3). To avoid sharp temperature differentials at the ends of the test section, the length of the furnace is four times the gauge length. Sixteen-inch coupons are used „ to reduce the temperature of the threaded joints and thus to facilitate removal from the grips. Thermal losses are minimized by refractory insulators cut to shape and surrounded by diatomaceous ear,th. The taps

Jan 1, 1942

By J. W. Spretnak, G. W. Powell, J. H. Bucher

Tlze room-temperature tensile fracture oj smooth, round specitnens of three ultrnhigh- strength steels tempered to a wide range of strength levels was studied by means by light and electron-microscopic examination of the fracture surfaces. The fracture of AISI 4340 and 300 M at all the strength levels studied, and H-11, except after tempering at 1200° and 1300°F, occurs in three stages. The initiation of fracture is internal (except in some lightly tcmpeved specimers in which fracture is initiated at surface flaws), and is nucleated largely by separation at metal-second phase intevjaces. TIze voids grow and, coalesce to form a crack. When the crack has reached a sufficienl size, rapid propngutio~z ensues. Failure in this stage of fracture usually occurs by dimpled rupture of inicroshear stefis. In the case of H-11 tempered in the 1125° to 1300°F range, fracture in the shear steps is predominantly by concentrated deformation without void formation. The termination of fracture is usually occomplished by the formation of a shear lib in which fracture occurs by shear dimpled rupture. In the case of H-11 tempered at 1200° and 1300°F, no shear lip was obserued, and the radial elelments extend to the surface—a true termination slage does not exist. ThE tensile fracture of several metals and alloys has been investigated.2-4 In the case of polycrystal-line materials, cup-cone fracture usually results. The mechanism of cup-cone fracture may be summarized as follows.5 Cavities are formed in the necked region of the specimen. They usually are initiated by inclusions or second-phase particles. The cavities extend outwards by means of internal necking, and a crack lying about perpendicular to the length of the specimen is formed in the necked region. Subsequent crack growth occurs by the spread of bands of concentrated plastic deformation inclined at an angle of 30 to 40 deg to the tensile axis. Cavities are formed in the bands of concentrated deformation. The deformation bands zigzag across the bar with the net result that mac-roscopically the crack extends about perpendicular to the specimen axis. The final separation, or cone formation, appears to occur by continued crack propagation along one of the deformation bands out to the surface of the specimen. The micromechanics of the tensile fracture of ultrahigh-strength steels have not been thoroughly investigated. Larson and carr6,7 studied the tensile-fracture surfaces of AISI 4340 with a low-power microscope and reported that three stages of fracture could be observed in general. A centrally located region characterized by circumferential ridges, an annular region characterized by radial surface striations, and a peripheral shear lip were found. It was first pointed out by 1rwin8 that the central region is very probably one of fracture initiation and slow growth, and that the annular, radially striated region is one of rapid crack growth. Presumably the crack grows slowly, assuming roughly a lenticular shape, until it is large enough for the initiation of rapid propagation. In this investigation, it was attempted to determine the fine-scale aspects of the room-temperature tensile fracture of some ultrahigh-strength steels, and to relate the variation in fracture mode with microstructure. The steels studied were AISI 4340, 300M, and H-11 tempered to a wide range of strength levels. I) EXPERIMENTAL PROCEDURE The compositions of the steels studied are given in Table I. The steel was received in the form of hot-rolled bar stock 5/8 to 1 in. in diameter from which oversized specimens were machined and heat-treated. The heat treatments employed are given in Table 11. Subsequent to heat treatment, the specimens were ground to the final dimensions and stress-relieved by heating for 1 hr at 350°F (with the exception of the as-quenched steel). Standard smooth round specimens of 0.252-in. diameter and 1-in. gage length were tested in a Tinius Olsen Universal Testing Machine using a cross-head speed of 0.025 in. per min. The relatively coarse aspects of the fracture topography were determined by light-microscopic examination of sections through the fracture surface of nickel-plated specimens. A direct carbon-replication technique9 was used in the electron-microscopic study of the fracture surfaces. The replicas were examined in the electron microscope, and stereo pairs of electron micrographs were taken. The stereo pairs were then examined using a Wild ST4 Mirror Stereoscope. Carbide and inclusion particles extracted in the replicas were analyzed by selected-area electron diffraction. II) EXPERIMENTAL RESULTS The mechanical testing data are summarized in Table 111. The values reported are the average of

Jan 1, 1965

By Samuel D. Warriner

(Wilkes-Barre Meeting, June, 1911.) THE dealings between concentrated capital invested in the conduct of our various industries and the combinations of labor known as "trade union organizations," have produced not only in the United States, but abroad, many novel methods of negotiation between employers and wage-workers. The size and strength of these organizations have destroyed the personal elements formerly governing the dealings between employer and employee and have produced various forms of trade-agreements now in more or less successful operation. The difficulty, however, has- been to secure consent of both parties to an equitable agreement. For this purpose there have been devised various forms of arbitration, either compulsory under the shadow of governmental legislation, or voluntary by mutual agreement. But these have not been altogether successful from a technical stand-point, for the reason that a compromise has generally been necessary, and in an effort to reach an agreement, terms have been made which have been neither fair nor satisfactory to either of the contending parties. The Anthracite Board of Conciliation represents one of the few thoroughly successful courts for the settlement of trade-disputes, if not the only one which has yet been evolved. The prestige of this board rests upon its successful treatment of the labor-troubles of the anthracite region for a period of more than eight years, and upon the fact that it has been able not only to reach decisions based upon the merits of the controversies, but to enforce its decisions upon both the employees and the employers. It has never been obliged to shape its conduct to secure the consent of the contending parties, and its decisions have been strictly and, in the main, cheerfully observed. The remarkable feature of this board has been that it has

Aug 1, 1911

By Kiyoshi Mizui

Processes for manufacturing prereduced iron pellets from iron ore dust occurring in iron works have recently begun on an industrial scale. Because of their high porosity and low mechanical strength, these prereduced iron pellets tend to oxidize again and disintegrate into fine particles during transportation and storage; this may result in such difficulties as decreased yield, undesirable work environment and heat generation during oxidation. A possible process for avoiding oxidation and disintegration of prereduced pellets is increasing the density through briquetting. The authors carried out briquetting tests under various conditions, attempting to find optimum briquetting conditions. They found that crushing prereduced pellets and adjusting the particle size to a certain range before briquetting increased the briquette strength and reduced the amount of binder needed. Oxidation resistance of briquettes and raw material pellets was compared in open air and at high temperatures. Briquettes showed superior oxidation resistance.

Jan 1, 1977

By Tasuku Fuwa, John Chipman, David H. Kirkwood

Fe-C-Si alloys in silica crucibles were held at 1600°C in a controlled atmosphere of CO and Co2 and the approach to equilibrium was obsertsed. Results were not of sufficient precision to establish the activity and interaction coefficients. Observations 012 the equilibrium provided an average value for the standard free-energy change which differed by + 1.1 kcal from the earlier accepted value. The C-SL relation at other temperatures is calculated and shown graphically. IN the refining of steel in an acid-lined furnace, it is well known that, unlike in basic refining, a very significant amount of silicon may remain dissolved in the metal even when the carbon content approaches a final endpoint. Further, it is known that the residual silicon increases with increasing temperature. The quantitative relation between silicon and carbon can be calculated for equilibrium conditions from data already available on the Fe-C-O and the Fe-Si-O systems. Such equilibrium calculations could show us approximately the limitations within which the reaction would be expected to operate in practice. In the oxidation of a bath containing both carbon and silicon it is well known that at low temperatures silicon is preferentially oxidized first. It can be shown by calculation that at high temperatures carbon will be oxidized preferentially. It is the purpose of this paper to record direct observations on the Si-C relation by means of experiments carried out in an atmosphere of carbon monoxide for Fe-C-Si alloys contained in silica crucibles. When such a system is brought into equilibrium, at a fixed temperature, the composition of the liquid metal is governed by the following equations: Both K1 and K2 are known with a fair degree of accuracy, and may be calculated from the tabulated In general the percentage of CO2 is extremely small compared to that of CO and in the experiments to be described the partial pressure of the latter was generally only slightly below 1 atm. EXPERIMENTAL METHOD The induction furnace employed was the same as that described by Rist and chipman&apos; and by Fuwa and chipman.2 It was modified slightly in view of the change from alumina to silica crucibles. The small silica crucible was surrounded by a thin susceptor of molybdenum sheet which in turn rested inside a zirconia crucible. Since the zirconia was subject to breakage, it was supported inside an alumina crucible. The charge consisted of 30 to 35 g of electrolytic iron along with the required amounts of refined silicon and graphite to produce a melt of required composition. Purified carbon monoxide and carbon dioxide were passed into the furnace through carefully calibrated flow meters. Two separate and independent series of experiments were carried out. In Series I (D.H.K.) the melt was held in the furnace at 1600°C for periods of time up to 6 hr. Samples were taken at intervals in silica tubes and were analyzed for carbon and silicon. The results of the last one or two samples taken from each experiment and the direction in which equilibrium appeared to be approached are shown in Table I. In Series II (T.F.) the silica crucibles were of less satisfactory strength and the melts were held at 1600° C for periods of only 2 to 4 hr. In heats number 29 to 45 inclusive, the metal was cooled in the furnace and the ingot itself served as a sample for analysis. In heat 46 and all subsequent heats, samples were withdrawn in silica tubes at the termination of the heat, and these samples were analyzed. The results of all of these experiments in which equilibrium appeared to be approached are listed in Table II.

Jan 1, 1965