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By E. P. Klier, Volker Weiss, George Sachs

IT has been shown that the isothermal transformation of austenite in a special steel can be modified by isothermal holding in the high subcritical transformation range.' Since this treatment potentially leads to increased hardenability, limited testing has been completed to determine if the stabilization effects observed with this treatment can be used to advantage in the heat-treating of 4340 steel. As an index of the effects of the several austenitizing treatments on the hardenability of the steel, Jominy-type hardenability tests were completed for specimens 2.5 in. in diameter and 8 in. long. Since the steel studied is to be used at strength levels where notch sensitivity is of major concern, notch sensitivity after selected austenitizing treatments has been evaluated by notch tensile tests for several specimen sizes. The steel composition and the austenitizing treatments are given in Table I. The test specimens are presented in Fig. 1. The hardenability data are given in Fig. 2 and the notch tensile properties are presented in Fig. 3. The hardenability of the steel investigated when determined by use of the standard Jominy test specimen2 as high and remained essentially unchanged for the different austenitizing treatments. For the larger test specimen, as has been shown by other investigations," the characteristic hardenability indexes are changed and it becomes possible to isolate austenitizing treatments which promote maximum hardenability. The stepped austenitizing treatment promotes higher hardenability as is indicated in Fig. 2. The evaluation of notch sensitivity for very high strength steels is best accomplished by means of the notch tensile test. The experimental conditions of the test, however, modify the notch strengths measured, and in the present experimentation an effort was made to achieve a limiting notch condition by fixing the notch root radius at 0.001 in. while the specimen diameter was allowed to increase from 0.3 to 1.1 in.* For this root radius the notch strength, 0.3-in.-diam specimen, and this trend differs from that for the larger specimens. At the highest tempering temperatures the 1.1-ip.-diam specimens yield comparable results for the austenitizing treatments compared. However, as the tempering temperature is progressively lowered below 800°F, em-

Jan 1, 1958

By R. M. Fowler, H. L. Hamner

DURING the last 25 years, there appeared in the literature a number of papers describing equipment and operating techniques for the determination of total oxygen in iron and steel. In the early papers, comparatively little attention was paid to side reactions that occur when iron is saturated with carbon at a high temperature in a high vacuum. As more experience was gained with the new method, the limitations appeared. Metals, with a boiling point lower than iron, distilled out of the crucible, condensed in the cooler part of the furnace, and subsequently reacted with carbon monoxide to form oxides and carbon. Aluminum, manganese, and the alkaline earth metals proved troublesome in this respect. Modifications have been devised to overcome the difficulties due to aluminum and manganese, while the alkaline earth metals are not of too much concern as yet to the steel chemist. The reactions of sulphur have received less attention, although it is generally recognized that some carbon disulphide is probably formed. Liquid air traps have been used in some cases to prevent any carbon disulphide from entering the analytical train. Sulphur was not a particular problem at the Union Carbide and Carbon Research Laboratories until the analysis of the irons of higher than usual sulphur contents became necessary. In order to describe the procedure developed for such irons, it will be necessary to first describe the type of vacuum-fusion equipment employed because the operation of vacuum-fusion equipment is an art to a considerable extent. At the Laboratories, vacuum-fusion equipment has been in daily operation since about 1930. Over the years, the evolution of this apparatus has been governed by the versatility required to analyze a wide variety of materials. Since all types of materials from high purity metals to slags are analyzed and, since seldom more than a few samples of one type are analyzed in succession, the apparatus was designed for accuracy and flexibility rather than for speed. A general view of the equipment is shown in Fig. 1, while Fig. 2 shows the relationship of the various parts. In Fig. 2, A is a vertical double-glazed 24X27/8 in. OD silica tube heated with a 20 kva mercury-arc high frequency generator. The tube is closed with a water-cooled brass head attached with de Khotinsky cement. A turret cap fits on this head and is sealed with a 1/8x3 in. "0" ring. The head contains a sight glass and two 8 in. horizontal glass tubes, for sample storage, cemented in with de Khotinsky cement. B is a four-stage Gaede mercury diffusion pump connected to the water-cooled head with a 11/2 in. copper tube through a flange with an "0" ring. The output of the vacuum pump feeds into an automatic Toepler F pump which compresses the gas sample over mercury in the measuring burettes, G and H. There are bypasses in this line for a McLeod gage C and a Piranni gage D, a manometer E, and for initial pumping out of the system with a Cenco Megavac backing-up pump. The reduction crucible shown in Fig. 3 is machined of Tungar Bulb quality (A.G.K.T.E.-2) graphite. The sample is guided into the crucible with the graphite funnel depicted on this figure. The arrangement of the crucible, radiation screens, etc. in the furnace is as follows: A 1 15/16x61/2 in. Alundum thimble, porosity RA-84, with two 1/8 in. holes near the top and opposite each other which take a pair of special tongs used for lowering it in place, is prepared. A 3/4 in. layer of powdered graphite is placed in this Alundum thimble, and the graphite crucible containing 20 g of ingot iron and 0.5 g of carbon is carefully centered on this bed of graphite powder and graphite powder is packed around it to the top of the graphite cru-

Jan 1, 1953

By A. H. Grobe, F. N. Rhines

AT elevated temperatures the oxide of silver is unstable in the air at atmospheric pressure, consequently no external oxide scale forms upon pure silver under conditions of high-temperature annealing When small quantities of certain alloying elements are present in the silver, the formation of a thin external scale is possible' and in addition there may form a subscale composed of the oxide of the solute element precipitated within the body of the silver Norbury2 and Leroux and Raub3 have reported internal oxidation (subscale formation) in alloys of silver with 2, 7 5, and 30 per cent of copper The presence of the subscale is believed to be responsible, at least in part, for the objectionable "fire mark" in Sterling silver' Several other alloys of silver, after oxidizing heat-treatments, are known to exhibit undesirable polishing characteristics that may be the result of internal oxidation Except for the absence of an external scale of silver oxide, it is to be anticipated that silver alloys will prove to be very similar in their oxidation behavior to the alloys of copper, the oxidation characteristics of which have been studied in some detail 5,6 The present research confirms this anticipation The oxidation of a series of 20 dilute alloys of silver has been studied metallographically, some types of subscale not encountered among the copper alloys have been found Instances of internal oxidation in alloys of most of the metals of the I-b and VIII groups of the periodic system are on record, but evidence of this type of oxidation in alloys of the metals of the intermediate groups is lacking A number of the metals of the intermediate group, among them cadmium, lead, tin, and zinc, appear to provide the conditions essential to subscale formation, i e , they form oxides with a relatively low negative free energy of formation, they dissolve other metals that form more stable oxides, and, presumably, oxygen will diffuse through them In a study of 4o alloys of these white metals only a few cases of internal oxidation have been found The probable reasons for this difference in behavior will be discussed presently EXPERIMENTAL PROCEDURE Silver -The silver alloys employed in the oxidation studies were prepared in heats of 30 grams each from high-purity silver (99 993 per cent Ag)* and the purest avail-

Jan 1, 1942

By William E. Bruce

In recent investigation of drilling processes, the U.S. Bureau of Mines measured the operating characteristics of two percussive drills. Basically, this entailed measuring maximum piston velocities while drilling. The maximum piston velocity is not necessarily the same as the striking velocity. The latter is usually somewhat lower1 because most commonly used drills provide an air cushion which slows the piston just before it comes in contact with the drill rod. Penetration rates for the two drills were determined in nine rock types, and the physical properties of the same nine rocks were measured and tabulated. Then the penetration rates were plotted against the individual properties to determine the general relationships on which methods for predicting drilling rates could be based.2

Jan 1, 1970

By Paul Foote

The temperature of a material may be ascertained by measurement of the intensity of the radiant energy it emits. This measurement may refer to the radiation of all wave lengths emitted by the material, or, if the material is glowing, the measurement may refer to the visible light emitted, or to the radiation in n very restricted portion of the visible spectrum. In general, the intensity of radiation depends not alone upon the temperature of the source, but, also upon its nature. Thus, glowing carbon appears to the eye about three times as bright as glowing platinum, at the same temperature. This is technically expressed by saying that the emissive power or emissivity of carbon is about three times that of platinum. A material having the highest theoretically possible emissivity is known as a "black body;" it is customary to assign a numerical value of 1 to the emissivity of a black body. A black body is experimentally realized by uniformly heating a hollow enclosure and observing the radiation coming from a small opening in the wall. The intensity of radiation emitted from this opening depends only on the temperature of the walls, and not on the material of which they are constructed. If E is the emissivity of any non-transparent material and R is its reflection coefficient, it can be shown that E + R, = 1. If a material having an emissivity of, say, 0.40, and hence a reflection coefficient of 0.60, is placed inside a black body it becomes indistinguishable from its Surroundings, because the total intensity of radiation leaving the material is the same as that emitted by the black body. While the material actually emits only 40 per cent of the intensity of a black body at the same temperature, 60 per cent. of the radiation falling upon it from the walls of the enclosure is reflected. However, if the material is removed from the black body and placed in the open air, the reflected intensity is no longer present and the object appears but 40 per cent. as bright as a black body at the same temperature.

Jan 8, 1919

By F. Paredes, W. R. Holman, R. W. Crawford

The diffusion coefficient for hydrogen in the ß titanium alloy containing 13 pct V, 11 pct CY, and 3 pct A1 was measured over the temperature range 20° to 500°C. Results fit the expression: D= 1.58 x lgs exp-------==-----) cm2,sec THE diffusion coefficient for hydrogen in the metastable ß-phase titanium alloy containing 13 pct V, 11 pct Cr, and 3 pct A1 was measured as part of an investigation of the effects of hydrogen on the mechanical properties of titanium alloys. Several theories on the mechanisms of hydrogen embrittle-ment include diffusion of hydrogen at ambient temperature as an important step in the embrittling process.'-5 In hydrogen-contaminated a-ß titanium alloys, it has been postulated that the rate-controlling step may be the rate at which hydrogen diffuses from the ß phase to stress- or strain-nucleated brittle hydride platelets at the a-ß interface.' However, embrittlement of the all-ß alloy investigated in this work may proceed by a different mechanism, since this alloy can be embrittled without the formation of detectable hydride platelets.6 Troiano has suggested that in this case the mechanism of delayed failure or embrittlement is similar to that proposed for high-strength steel, i.e., repeated crack initiation caused by a decrease in bonding energy as hydrogen diffuses to points of high tri-axial stress at the root of a notch. In both types of alloy the rate of embrittlement is believed to be controlled by diffusion of hydrogen in the ß phase. Accurate hydrogen-diffusion data in the vicinity of room temperature should therefore be of some assistance in understanding the mechanisms of embrittlement in these two classes of titanium alloys. Diffusion of hydrogen in pure titanium has been studied by Wasilewski and Kehl7 at temperatures above 500°C. Their measurements on diffusion in the ß phase were extended below the ß-a transformation temperature (882°C) to approximately 600°C. This was possible because of the 8 stabilizing effect of hydrogen. No results at lower temperatures have been published and there are no data in the literature on hydrogen diffusion in the ß -phase alloy used in this program. Hydrogen diffusion in metals is generally investigated by measuring the rate of transport of hydrogen past a solid-gas interface, i.e., by absorption, permeation, or degassing-rate measurements. These methods produce accurate diffusion data when bulk diffusion is the rate-determining step in the over-all process. However, at the lower temperatures of interest in hydrogen-embrittlement studies or under conditions where surface films are present, the measured rates may be surface-controlled and the calculated diffusion coefficients will be in error. Surface effects were eliminated in the present work by using a modification of the common welded-couple technique m which two bars with uniform but different compositions are joined before the diffusion anneal." The same type of step change in the initial concentration vs distance curve was produced by electrolytically hydrogenating thin-strip specimens which had been electrically insulated over half of their length. Concentration vs distance curves were determined, after appropriate diffusion-annealing treatments, by vacuum-extraction analyses of transverse samples sheared from the strips. Diffusion coefficients were calculated by the methods of Grube.M This technique was feasible because of the large concentrations of hydrogen which can be charged into p -phase alloys without the formation of hydrides15'16 and because of the extremely low degassing rates observed when hydrogenated titanium alloys are heated in air. EXPERIMENTAL WORK The diffusion couples were cut from a 0.022-in.-thick mi ll-annealed sheet.* Strips 8 in. long by 1/2

Jan 1, 1965

By S. S. Hartranft

FuRnace-men of the present day agree very nearly as to the best cooling-devices for the protection of blast-furnace hearths and boshes, and the best location of the cooling-system in the brick-work for the maintenance of favorable furnacelines throughout the blast. The replaceable bronze and copper plates are practically faultless; and there seems to be no reason why a furnace-hearth and bosh should not be held in good condition, by intelligent management and the use of replaceable plates, for a period several times the length of the average blast of to-day. While furnace-men have taken these .precautions to protect the hearth and bosh beyond the life of the lining, the portion of the lining above the mantle has been partly protected by some and wholly neglected by others. Some would not construct a furnace without mantle-plates, and others would not construct a furnace with them. In most cases, furnace-men have either trusted to Providence or to the bosh-plates for the continuance of favorable working-conditions above the mantle, and the prolongation of the life of the lining; consequently furnaces are constantly blown out for repairs to the lining, or for relining, when the hearth and bosh are in good enough condition to last through another blast. The following extract from one of Mr. James Gayley's con-

Jan 1, 1901

By John Griffen

This paper records over twenty years' experience with the use of the Rheolaveur system in the United States, showing its ability to meet changing conditions caused by the dirtier mine output of present-day mechanical mining methods. Data are given on size ranges handled, number and capacity of units installed, maintenance experience, and operating results on two-product and three-product separations. IT is not the purpose of this paper to discuss the principles employed in the Rheolaveur system of fine-coal cleaning as these have been fully covered in the technical literature of the Institute."2 Rather, our purpose will be to record the highlights of over 20 years' experience in the United States with Rheolaveur fine-coal launders, which will indicate their capabilities and costs of cleaning and their adaptability to meet the changing conditions caused by present-day mechanical mining methods. Rheolaveur fine-coal launders are used in the United States to treat a wide variety of size ranges of fine coal, the coarsest being 1/2 in. to 0 and the finest about 1/8 in. to 0. In Europe feeds as coarse as 5/8 in. and as small as 1/2 mm (28-mesh) to 0 are being cleaned. The size ranges usually handled in this country are 3/8 to 1/4-in. round to 0. Thirty five units with a combined hourly feed capacity of 3200 tph have been installed in the United States. Individual units are cleaning as little as 25 tph, while others are cleaning as much as 200 tph. Rheolaveur fine-coal launders offer cleaning units of high capacity and are outstanding in requiring a minimum of building space per ton of input. Experience has shown that maintenance costs are low. Several installations were made in the Pittsburgh district from 1928 to 1930, and since that time operation has been largely two shifts per day. Minor repairs to liner plates and Rheo boxes have been required during the intervening years, but no major replacement of launders was required until 1947 and 1948. At one of these plants, launders operated for 17 years before they were replaced and during that period over 26,000,000 tons of —5/16-in. coal were cleaned. The effect of the much dirtier raw coal produced by mechanical loading of the Pittsburgh seam is shown by the following tests. The data in table I summarize the performance of a Rheo fine-coal unit when cleaning hand-loaded raw coal. The —4-in. raw coal fed to the cleaning plant analyzed only 8.16 pct ash and 1.31 pct sulphur and contained 4.6 pct sink, 1.55 sp gr. Two years later, in 1945, mechanically-loaded coal from the same mine was cleaned in the same plant. The feed, —4 in., then analyzed 20.10 pct ash and 1.53 pct sulphur and contained 20.2 pct sink, 1.55 sp gr. The performance of the Rheo fine-coal unit when cleaning this coal is given in table 11. It will be noted that the +48-mesh coal is cleaned almost as thoroughly as in table I. The large amount of high-ash slimes produced from the dirtier feed are responsible for the higher ash of —--48-mesh washed coal in table 11. In this plant the Rheo fine-coal unit did not get the full load of refuse resulting from mechanical

Jan 1, 1951

By John Griffen

This paper records over twenty years' experience with the use of the Rheolaveur system in the United States, showing its ability to meet changing conditions caused by the dirtier mine output of present-day mechanical mining methods. Data are given on size ranges handled, number and capacity of units installed, maintenance experience, and operating results on two-product and three-product separations. IT is not the purpose of this paper to discuss the principles employed in the Rheolaveur system of fine-coal cleaning as these have been fully covered in the technical literature of the Institute."2 Rather, our purpose will be to record the highlights of over 20 years' experience in the United States with Rheolaveur fine-coal launders, which will indicate their capabilities and costs of cleaning and their adaptability to meet the changing conditions caused by present-day mechanical mining methods. Rheolaveur fine-coal launders are used in the United States to treat a wide variety of size ranges of fine coal, the coarsest being 1/2 in. to 0 and the finest about 1/8 in. to 0. In Europe feeds as coarse as 5/8 in. and as small as 1/2 mm (28-mesh) to 0 are being cleaned. The size ranges usually handled in this country are 3/8 to 1/4-in. round to 0. Thirty five units with a combined hourly feed capacity of 3200 tph have been installed in the United States. Individual units are cleaning as little as 25 tph, while others are cleaning as much as 200 tph. Rheolaveur fine-coal launders offer cleaning units of high capacity and are outstanding in requiring a minimum of building space per ton of input. Experience has shown that maintenance costs are low. Several installations were made in the Pittsburgh district from 1928 to 1930, and since that time operation has been largely two shifts per day. Minor repairs to liner plates and Rheo boxes have been required during the intervening years, but no major replacement of launders was required until 1947 and 1948. At one of these plants, launders operated for 17 years before they were replaced and during that period over 26,000,000 tons of —5/16-in. coal were cleaned. The effect of the much dirtier raw coal produced by mechanical loading of the Pittsburgh seam is shown by the following tests. The data in table I summarize the performance of a Rheo fine-coal unit when cleaning hand-loaded raw coal. The —4-in. raw coal fed to the cleaning plant analyzed only 8.16 pct ash and 1.31 pct sulphur and contained 4.6 pct sink, 1.55 sp gr. Two years later, in 1945, mechanically-loaded coal from the same mine was cleaned in the same plant. The feed, —4 in., then analyzed 20.10 pct ash and 1.53 pct sulphur and contained 20.2 pct sink, 1.55 sp gr. The performance of the Rheo fine-coal unit when cleaning this coal is given in table 11. It will be noted that the +48-mesh coal is cleaned almost as thoroughly as in table I. The large amount of high-ash slimes produced from the dirtier feed are responsible for the higher ash of —--48-mesh washed coal in table 11. In this plant the Rheo fine-coal unit did not get the full load of refuse resulting from mechanical

Jan 1, 1951

This paper "On Coal" was published in three issues of The Western Gleaner in 1814. Name of author is not given. This magazine was started by Cramer, Spear & Eichbaum, in Pittsburgh, Pa., in December 1813, and ran for about two years. Copies are very rare, and this one is made from an original in the Darlington Library, University of Pittsburgh. This is almost certainly the first general article on coal published west of the Allegheny Mountains, and one of the earliest in this country. ON COAL Its Natural History-Mining of Coal-Phenomena occasioned by Fire-damp-Method of Coking-Distillation of Tar from Pit-coal-Gas-light-Coal, a Manure I. NATURAL HISTORY OF COAL There are few productions of nature which present to the philosopher a wider field of investigation than pit-coal. A substance highly inflammable is found in the deep recesses of the earth, sometimes loaded with numerous superincumbent strata of hard rock, and extending frequently along with these strata through a vast expanse of territory. Though metals may be said to be inflammable substances, as they combine more or less rapidly with oxygen when placed under particular circumstances, yet the character of rapid combustion with disengagement of light and heat, seems to belong. principally to such substances as are derived either from the animal or vegetable kingdom. That this is probably the case with regard to coal we are further induced to believe, by the remarkable circumstance, that the chemical analysis of this natural production yields especially, though in various proportions, those materials which constitute essentially the vegetable. And if any thing was wanting to confirm, us in that opinion we might trace in a number of fossile substances the gradual transition of the vegetable into the state of mineral coal. This fact is so intimately connected with the natural history of coal, that we cannot think it superfluous to give it some farther development. Among the great number of principles which the chemist is capable of tracing in the vegetable kingdom, the presence of extract, resin and fibre seem to form the characteristical marks of plants.-If vegetable matter be boiled in water, and the water, after having been strained and filtered, be exposed for some time to the open air, a flocculent precipitate takes `place from every part of the liquor; which soon subsides to the bottom of the vessel containing it. This is the extract; altered, indeed, by exposure, and now no longer soluble in water, a change which is supposed to depend on the absorption of oxygen; and if, by any means the proportion of oxygen be increased, the extract gradually becomes of a darker color, blackens, and approaches to the state of charred wood.

Jan 1, 1942

By Chester O. Ensign

Many publications to date have advocated under- seas mining operations, optimistically overlooking the paucity of information on mineral distribution and the ocean environments in which minerals occur. Such articles (smattered with opinion, as is this article) are herein tempered by my more conservative views on the economics of mining under the seas. For purposes of this paper, underseas mining refers only to the deeper surficial deposits of the continental shelf and the deep sea floor, i.e., the deposits of phosphorite and manganese nodules.

Jan 9, 1966

By P. Ramachandraraa, T. R. Anantharaman

THE technique developed by Duwez, Willens and Kle-ment' for rapid solidification of molten alloys in small quantities by ejecting them on to a highly conducting substrate with the aid of a shock wave has come to be known as "liquid quenching" or "splat cooling" in literature and has already been applied to alloys of many binary systems.' The very high cooling rates of the order of l060 to 1080 per sec obtained in this technique and the consequent drastic undercooling of the melt have led to such striking results as formation of new amorphous and crystalline metastable phases and extension of solid-solubility limits in many alloy systems. The cooling rates in these experiments can, however, be neither accurately measured nor effectively controlled and hence the occurrence of either more than one metastable phase or appreciable differences in constitution in splat-cooled alloys of the same composition cannot be ruled out.3 In fact, workers in two laboratories have reported formation of two different cubic metastable phases in liquid-quenched Au-Si alloys containing 17 to 20 at. pct si.4,5 The present note deals with some new and interesting results obtained in a Ag-21 at. pct Ge alloy and a Au-27 at. pct Ge alloy subjected to the liquid-quenching treatment at different cooling rates. Two alloys of nearly the same composition had earlier been rapidly solidified by the standard "gun technique" in the same laboratory and shown to solidify in nonequilibrium structures, viz., an hcp phase (a = 2.987Å;c =4.718Å) in the Ag-Ge system6,7 and both hcp (a = 2.885Å; c = 4.754Å) and tetragonal (a = 11.627A; c = 22.491Å) phases in the Au-Ge system.3 Apart from different substrates (copper and stainless steel), different melt temperatures (50º to 500°C above the liquidus), and different capillary sizes (0.4 to 1.5 mm diam) in the "gun technique", slower cooling rates of the order of l050C per sec were also obtained in the present work by replacing the substrate by water at room temperature in a modification of the technique due to Olsen and Hultgren.8 No attempt was made to measure the cooling rate in any experiment. The products varied from fine powder (>40 pct by wt—200 mesh) obtained by quenching in water to thin flakes and foils (11.0 sq mm to 4.0 sq cm) produced by splat cooling. They were subjected to the Debye-Scherrer method of X-ray examination in each case. In case of the Ag-Ge alloy, in addition to the expected metastable hcp phase,6 a coexistent tetragonal phase (a = 5.093,Å; c = 7.009Å) was detected in some experiments. Eight weak X-ray reflections from this phase could be identified, two of them being the same as reported earlier.7 With increase in the cooling rate, the dominant hcp phase seems to be first accompanied by traces of silver or germanium and then either homogeneous or mixed with traces of this new tetragonal phase. The splat-cooled Au-Ge alloy showed generally the expected hcp and tetragonal phases,3 but sometimes traces of germanium were also present. Further, two new tetragonal phases with the following lattice param ters could be clearly identified in samples quenched

Jan 1, 1970

(Under this heading will be published notes sent to the Secretary of the Institute by members or other persons introduced by members) Member, Graduate Colorado School of Mines. Four years' experience in West and Northwest. Two years with American Smelting and Refining Co. Wishes to join field party on geological work, mining or areal, where opportunity will be given to be of direct assistance to chief of party in solution of field problems. Age, 26. Unmarried. At liberty June 1. No. 342. Member, technical graduate, aged 30, with' 7 years' experience in concentrating and mining, desires a position of authority with reliable company. At present employed. No. 343. Member. Ambitious, energetic, tactful engineer, college graduate, married, aged 30, desires location with a large coal mining organization. Seven years with present employers -n middle west; has had broad experience in the past eight years on examination, development and construction; successful record in handling men. Position must carry responsible work and a future. Will go anywhere for proper opportunity. Exceptional references as to reliability, character and capacity for work. No. 344.

Jan 3, 1917

ARTHUR CROWFOOT, Morenci, Ariz. (communication to the Secretary*).-In order to set at rest any doubts in regard to the reasons for selecting the Callow pneumatic flotation process for use in the concentrators of the Arizona Copper Co., Ltd., at Clifton and Morenci, I am presenting the following facts gained from the results of test work carried out on the Callow and Cole-Bergman types of flotation machines at Morenci. Prior to the comparative test of merit between the Callow and Cole-Bergman machines, many months' time and a large amount of money had been expended in the development and testing of the Cole-Bergman machine, and it was necessary to decide quickly what make of machine was best to install. The Callow pneumatic flotation process was recommended for installation in our concentrators for the following reasons: The results indicated: 1. That the Callow system made the highest extraction of copper values from the feed treated. 2. That the Callow system was simpler to operate and could he operated it a lower cost. 3. That the Callow system operated with a lower air pressure. (The question of the actual power consumption of the two types of machines was not definitely settled at this time.) During the official test period the Callow flotation apparatus showed an additional recovery of from 1 to 1.5 lb. of copper per ton more than the Cole-Bergman machine, this difference being maintained by further treatment of the tailing from both machines. The simplicity of the operation of the Callow flotation system is one of its notable features, two operators per shift being able to handle 90 standard cells and blower equipment.

Jan 7, 1917

By M. G. Driessen, H. E. Criner

Possible applications of cyclone thickeners for: (1) clarification of the washery water and, (2) recovery of fine coal from the plant bleed. The paper shows: (1) that it is possible to remove all particles including the very finest, from the circulating water, thus obtaining a closed water system and, (2) that reduction of the ash content of the solids of the plant bleed is feasible by means of cyclone thickeners. Performance data for different size cyclones is given in the form of graphs.

Jan 1, 1950

By Henri S. Swolfs

INTRODUCTION In this paper we present preliminary results of a research program in site characterization methodology. We are interested in under- standing the response of discontinuous rock to mechanical, hydrologic, and thermal loadings. To carry out such a study we selected a field site with simple geology, uniform distribution of lithologies, and easily verifiable boundary conditions on temperature, fluid flow and stresses. The spatial distribution of fractures at the site was established and tests were conducted to determine the temperature field, hydrology, rock-mass properties, and in situ stresses. As part of the study selected borehole instruments were compared to assess their performance and reliability. SITE GEOLOGY The study area is in the eastern part of South Table Mountain, a mesa near Golden, Colo. The exposed cap rock is a single lava flow of uniform thickness (6-7 m) that rests on the clastic sediments of the Denver Formation (Van Horn, 1976). The surface of the cap rock (N. 75º E., 3º S.) is topographically featureless and slopes south- southeast; drainage is predominantly downdip and punctuated by occasional contact springs. The age of the lava flow is 64-65 m.y., or early Paleocene. Paleo- botanic evidence confirms the upper part of the Denver Formation as Paleocene (Van Horn, 1976). "Rapid-rock" analyses of core samples from the lava flow at three depths (0.2, 3.3, and 5.8 m) suggest a uniform chemical composition throughout with an increase in the Fe2O3/ FeO ratio (1.05 to 1.60) with increasing depth, reflecting the existence of a perched water table in the lava flow, To identify the rock

Jan 1, 1984

By W. M. Reilly, Martin E. True, O&apos

A technique, equipment, and a compound have been developed and field tested for sealing tubing joint thread leaks without removing the tubing from the well. This eliminates the necessity of killing the well with possible damage to the producing formation, which could result if it were exposed to drilling mud. A thread sealing compound, developed and tested in the laboratory, is introduced into the tubing and squeezed into the joint to eliminate the leak. A high percentage of successful field applications have eflected an appreciable cost reduction in repairing leaking tubing strings in East Texas and in the Louisiana Gulf Coast area. INTRODUCTION In producing oil and gas wells the industry has been plagued with a never ending problem of tubing connection leakage. This situation is becoming increasingly more significant as more gas wells are placed on production and as higher pressures are encountered at greater depths of current drilling. Substantial progress has been made in minimizing thread leaks by careful handling and cleaning of joints and by the use of improved sealing compounds in combination with controlled makeup. But even with the use of the best known methods and sealing materials during initial makeup, occasional leaks through tubing joint threads appear inevitable. In some instances, tubing joints in high-pressure gas wells have been found to leak gas at relatively less pressure than that at which the tubing had been tested satisfactorily using liquid. Many expedients have been employed to prevent the physical replacement of tubing when leaks have developed. Perhaps the most commonly used is the sodium silicate treatment in which the solution is lubricated into the tubing to form a crystalline plug in the leak. Generally, any benefit realized is of a temporary nature. In addition to field studies on handling and makeup of tubing, extensive laboratory work has been undertaken on the development and testing of thread dopes.' Also, substantial effort has been devoted to testing tubing joints using high-pressure gas as a pressure medium.' The results of this work have emphasized that tubing joints are susceptible to occasional leaks, especially when subjected to relatively high differential pressures. To cope with the problem of leaking connections, an extensive investigation was undertaken to devise means of sealing leaks without removing the tubing from the well and without reducing the inside diameter of the tubing. The purpose of this paper is to present a technique, together with the associated equipment and compound, which have been developed for effecting a seal of leaking tubing in place. DISCUSSION Work was initiated simultaneously on two ventures: (1) to develop a satisfactory leak sealing compound and (2) to develop tools necessary to find the leak and place the compound. Leak Sealing Compound In the development of a sealing compound, tests were conducted on those compounds commercially available which include: (1) conventional thread lubricants, (2) thermo-setting resins and (3) other materials which held promise of effecting a seal. Although none proved completely satisfactory in their available form, two commercial compounds proved nearly equally effective in sealing leaks during laboratory tests after proportioned quantities of graded silica had been added. Field usage has indicated that the preferred compound is one prepared of an aluminum-stearate base thinned to the proper constituency and carrying a mixture of fine mesh graphite and graded silica. The compound developed by Humble Oil & Refining Co. is designated as Tubing Thread Leak Sealant 800. Placement Tools and Technique In developing tools to detect joint leaks and to place the sealing compound, work was done initially on wireline equipment. Preliminary designs were completed of a tool somewhat on the order of a pressure bomb to test individual joints with gas at high pressure to determine if the joint was leaking. An entirely different tool equipped with opposed packers was intended for placement of the sealing compound at high pressures in each leaking joint. The application of these tools

Jan 1, 1958

By A. Y. Bethune, W. G. Woolf

THE hydrometallurgy of special high-grade zinc as practiced by the Sullivan Mining Co. at its electrolytic zinc plant, Kellogg, Idaho, involves an important filtration step immediately following the leaching process. By means of the filtration the heavy zinc sulphate solution is separated from the residual products which remain after the zinc calcine has been dissolved in the sulphuric acid electrolyte. Because this plant uses the so-called high-acid, high-density process' for the production of First, the strength of the electrolyte (270g H,SO, per liter) results in a saturated zinc sulphate solution, having a specific gravity of 1.510 to 1.540, which must be kept warm during filtration because of its property of "seeding out" small crystals if allowed to drop much below 60°C. Second, the action of the "high" acid on zinc calcine under the temperature conditions of the leach (80" to 102 "C), although favorable to good zinc extraction, causes a considerable quantity of iron to be dissolved (8 to 18. g per liter) along with variable quantities of alumina and silica, depending on the grade and type of original zinc concentrates roasted. These three, iron, alumina, and silica, are almost completely precipitated during the neutralization of the leach (only a few. milligrams per liter of each remain in solution), so that the resulting pulp, instead of being a granular, sand-like product having a particle-size distribution dependent on the fineness of the zinc calcines leached, is in reality a slimy, chemical precipitate whose filtration characteristics constantly change depending on the amounts of iron silica, and other impurities, which are dissolved and reprecipi-tated. Third, the combination of supersaturated solution of high specific gravity plus a dense, semi-gelatinous residue creates a difficult washing problem requiring a positive displacement wash to liberate the zinc sulphate entrapped in the pulp. In a closed-cycle hydrometallurgical operation, such as practiced in this plant, the extent of washing is determined by the volum,e limitations imposed on the intermediate wash waters by the amount of "fresh" (or process) water which may be added. The volume of fresh water used for makeup purposes is limited to the amount which is lost during the closed cycle by evaporation in the leach, sulphate content of the calcines leached, moisture content of the residue, and spillage. The Burt filter as modified and improved by the Sullivan Mining Co. has successfully met and overcome these difficulties under a variety of zinc plant operating conditions since 1928. It might have many interesting applications to metallurgical fields other than that of electrolytic zinc, and its possible usefulness to hydrometallurgists in general warrants its description and discussion. The Burt filter is so named from its inventor who originated it in Mexico for pulp filtration in the cyanide process for gold and silver ores. While retaining the basic principle of Burt's earlier revolving pressure-type filter with internal filtration media, a number of modifications and improvements have been made in Sullivan Mining Co.'s installation. The Burt filter may be classified as a batch-type pressure filter in contradistinction to either the conventional vacuum-type filter, which depends on atmospheric pressure to force solution through a cloth medium, or to the filter-press, which employs whatever pressure is imparted by the pump delivering the liquid being filtered. The Burt consists essentially of a hollow steel cylinder about 40 ft long, 5 ft in diameter, resting horizontally, and capable of rotation about its long axis. It is supported on one end by a hollow trunnion and near the other end by a riding-ring and roller combination. The cylinder is lined with filter units each fastened against the inside of the shell and parallel to the long axis so as to form a hollow cavity into which pulp may be charged. A specific amount of pulp is admitted to the filter and a unique valving arrangement prevents the loss of pulp while air pressure forces the solution through a canvas medium to the discharge port of each filter unit. The residue is left on the surface of the canvas inside the cavity. The remainder of the filter cycle is concerned with washing the residue free of zinc sulphate, discharging it from the Burt, and preparing the filter for the next charge. A more detailed description of Burt filter construction, a typical filter cycle, and its operating characteristics when employed on material encountered in this plant will be given in that order. Description of the Filter: Fig. 1 shows a side elevation view of a filter with riveted shell construction. Since this drawing was made shells have been fabricated by welding, instead of riveting, with complete success. Shells are lagged on the outside to retain heat. Fig. 1 shows a side elevation and plan view of a Burt filter in operating position. The 1/2-in. steel shells are lined with 3/16-in. copper sheet as protection against the corrosive action of the solution (containing about 500 mg Cu per liter) on iron, and the copper is given a thin protective coating of plastic-base paint. Fig. 2 is a view from the discharge end of the filter, with head removed, before filter units are fastened to the periphery. It shows

Jan 1, 1951

By W. G. Woolf, A. Y. Bethune

THE hydrometallurgy of special high-grade zinc as practiced by the Sullivan Mining Co. at its electrolytic zinc plant, Kellogg, Idaho, involves an important filtration step immediately following the leaching process. By means of the filtration the heavy zinc sulphate solution is separated from the residual products which remain after the zinc calcine has been dissolved in the sulphuric acid electrolyte. Because this plant uses the so-called high-acid, high-density process' for the production of First, the strength of the electrolyte (270g H,SO, per liter) results in a saturated zinc sulphate solution, having a specific gravity of 1.510 to 1.540, which must be kept warm during filtration because of its property of "seeding out" small crystals if allowed to drop much below 60°C. Second, the action of the "high" acid on zinc calcine under the temperature conditions of the leach (80" to 102 "C), although favorable to good zinc extraction, causes a considerable quantity of iron to be dissolved (8 to 18. g per liter) along with variable quantities of alumina and silica, depending on the grade and type of original zinc concentrates roasted. These three, iron, alumina, and silica, are almost completely precipitated during the neutralization of the leach (only a few. milligrams per liter of each remain in solution), so that the resulting pulp, instead of being a granular, sand-like product having a particle-size distribution dependent on the fineness of the zinc calcines leached, is in reality a slimy, chemical precipitate whose filtration characteristics constantly change depending on the amounts of iron silica, and other impurities, which are dissolved and reprecipi-tated. Third, the combination of supersaturated solution of high specific gravity plus a dense, semi-gelatinous residue creates a difficult washing problem requiring a positive displacement wash to liberate the zinc sulphate entrapped in the pulp. In a closed-cycle hydrometallurgical operation, such as practiced in this plant, the extent of washing is determined by the volum,e limitations imposed on the intermediate wash waters by the amount of "fresh" (or process) water which may be added. The volume of fresh water used for makeup purposes is limited to the amount which is lost during the closed cycle by evaporation in the leach, sulphate content of the calcines leached, moisture content of the residue, and spillage. The Burt filter as modified and improved by the Sullivan Mining Co. has successfully met and overcome these difficulties under a variety of zinc plant operating conditions since 1928. It might have many interesting applications to metallurgical fields other than that of electrolytic zinc, and its possible usefulness to hydrometallurgists in general warrants its description and discussion. The Burt filter is so named from its inventor who originated it in Mexico for pulp filtration in the cyanide process for gold and silver ores. While retaining the basic principle of Burt's earlier revolving pressure-type filter with internal filtration media, a number of modifications and improvements have been made in Sullivan Mining Co.'s installation. The Burt filter may be classified as a batch-type pressure filter in contradistinction to either the conventional vacuum-type filter, which depends on atmospheric pressure to force solution through a cloth medium, or to the filter-press, which employs whatever pressure is imparted by the pump delivering the liquid being filtered. The Burt consists essentially of a hollow steel cylinder about 40 ft long, 5 ft in diameter, resting horizontally, and capable of rotation about its long axis. It is supported on one end by a hollow trunnion and near the other end by a riding-ring and roller combination. The cylinder is lined with filter units each fastened against the inside of the shell and parallel to the long axis so as to form a hollow cavity into which pulp may be charged. A specific amount of pulp is admitted to the filter and a unique valving arrangement prevents the loss of pulp while air pressure forces the solution through a canvas medium to the discharge port of each filter unit. The residue is left on the surface of the canvas inside the cavity. The remainder of the filter cycle is concerned with washing the residue free of zinc sulphate, discharging it from the Burt, and preparing the filter for the next charge. A more detailed description of Burt filter construction, a typical filter cycle, and its operating characteristics when employed on material encountered in this plant will be given in that order. Description of the Filter: Fig. 1 shows a side elevation view of a filter with riveted shell construction. Since this drawing was made shells have been fabricated by welding, instead of riveting, with complete success. Shells are lagged on the outside to retain heat. Fig. 1 shows a side elevation and plan view of a Burt filter in operating position. The 1/2-in. steel shells are lined with 3/16-in. copper sheet as protection against the corrosive action of the solution (containing about 500 mg Cu per liter) on iron, and the copper is given a thin protective coating of plastic-base paint. Fig. 2 is a view from the discharge end of the filter, with head removed, before filter units are fastened to the periphery. It shows

Jan 1, 1951

By C. H. Samans, G. F. Tisinai, J. K. Stanley

The addition of nitrogen (0.10 to 0.20 pct) to Fe-Cr-Ni alloys of simulated commercial purity results in a real displacement of the u phase boundaries to higher chromium contents. The effect is small for the (Y + s)? boundary, but is pronounced for the (y + a +s)/(y + a) boundary. Although there is an indication of an exceptionally large shift of the n boundaries to higher chromium contents, especially in steels with nitrogen over 0.2 pct, the major portion of this apparent shift results from the fact that carbide and nitride precipitation cause "chromium impoverishment" of the matrices. The effect of combined additions of nitrogen and silicon to the Fe-Cr-Ni phase diagram is demonstrated also. Nitrogen can nullify the effect of about 1 pct Si in shifting the (y + o)/? phase boundary to lower values of chromium at all nickel levels from 8 to 20 pct. NItrogen can nullify this U-forming effect of about 2 pct Si at the 8 pct Ni level, but not at the 20 pct Ni level. The alloys studied were in both the cast and the wrought conditions. There are indications that the u phase forms more slowly in the cast alloys than in the wrought alloys if both are in the completely austenitic state. The presence of 6 ferrite in the cast alloys accelerates the formation of U. Cold working increases the rate of o formation in both cast and wrought alloys. THE major improvement in Fe-Cr-Ni austenitic alloys in recent years has been in the addition or removal of minor alloying elements to facilitate better control of corrosion resistance, sensitization, and heat resistance. One shortcoming of the austenitic Fe-Cr-Ni alloys, which never has been completely circumvented, is their propensity toward u formation. In the AISI-type 310 (25 pct Cr-20 pct Ni) and type 309 (25 pct Cr-12 pct Ni) steels, sufficient amounts of u phase can form, if service or treatment is in a suitable temperature range, to cause severe embrittlement. Also, there is a growing conviction that this phase may be contributory to some unexpected decreases in the corrosion resistance of certain of the 18 pct Cr-8 pct Ni-type steels. The present paper discusses the effect of nitrogen additions on the location of the (r+u)/d and the (y+a+u)/(y+a) phase boundaries in the ternary Fe-Cr-Ni system, for cast and wrought alloys of simulated commercial purity, and in similar alloys containing up to about 2.5 pct Si. The objective is to define compositional limits for alloys which will not be susceptible to u formation when used near 1200°F (650°C). An excellent review of the early studies of the u phase in the Fe-Cr-Ni system has been compiled by Foley.1 Rees, Burns, and Cook2 have determined a high purity phase diagram for the ternary system, whereas Nicholson, Samans, and Shortsleeve3 are- stricted themselves to a portion of the simulated commercial-purity phase diagram. Both groups of investigators show almost an identical position for the commercially significant (y+u)/y phase boundary. Further comparison of the work of the two groups indicates that, below the 8 pct Ni level, the commercial alloys have a decidedly greater propensity toward u formation than the high purity alloys. The two groups of workers agreed that both the AISI-type 310 (25 pct Cr-20 pct Ni) and the type 309 (25 pct Cr-12 pct Ni) steels are well within the (y+~) region and that the 18 pct Cr-8 pct Ni-type alloys straddle the U-forming phase boundaries. Nicholson et al.3 showed, in addition, that these boundaries shift toward lower chromium contents if greater than nominal amounts of silicon or molybdenum are added. The effect of nitrogen on the location of the s phase boundaries in the Fe-Cr-Ni system has not been known with any certainty. In 1942, an approach to this problem was made by Krainer and Leoville-Nowak,' but at that time they apparently were unaware of the slow rate of s formation in strain-free samples and aged their samples for insufficient times, e.g., 100 hr at 650°C (1200°F) and 800°C (1470°F). For this reason, it would be expected that their (y+ u) /y boundary would be shifted toward lower chromium contents (restricted ?-field) when equilibrium conditions were approximated more closely. Procedure for Studying the Alloys The alloys used were prepared in the following way: Heats of 200 lb each were melted in an induction furnace. A 5 lb portion of each heat was poured into a ladle containing an aluminum slug for de-

Jan 1, 1955