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By A. H. Larson, R. J. McClincy

The activity of Sb,03 in PbO-Sb,03 slags containing less than 50 mol pct Sb,03 was determined by the inert-gas saturation method at 700°C. In this composition range, the activity gf SbzO3 shows a strong negative deviation from ideality. The activity of PbO in these slags was calculated by application of the Gibbs-Duhem iniegration to the Sb203 activity data. The calculated activity of PbO in slags containing more than 63 mol pct PbO was found to deviate in a positive direction from ideality uthile a negative deviation was found for slags containing less PbO. The standard Gibbs free energies of formation of Sb,03 and PbO. Sb203 have been calculated and compared with existing data in the literature. The activity of Sb203 in PbO-Si0,-Sb203 (PbO/SiO, = 2) slags containing less than 25 mol pct Sb,03 was also determined by the inert-gas saturation method at 700°C. In this composition range, the activity of Sbz03 shows a very large negative deviation from ideality. VERY little experimental work has been published in the past to determine equilibrium data in the oxide systems connected with the refining of lead. These data are of value since impurities such as antimony, arsenic, and tin must be removed from lead and recovered for further treatment. Equilibrium studies on antimony and arsenic systems are also of interest for the design of new processes for lead refining and lead dross treatment. Maier and ~incke' first determined the liquidus curves for the PbO-Sb203 system and identified the compound PbO . Sb203. They found the phase diagram for this system to be two simple eutectics located on either side of the congruent melting compound. They also determined a very limited amount of vapor pressure data for Sb406 abbve PbO-Sba3 melts at 697"~. A second phase diagram investigation on this system was reported by Hennig and Kohlmeyer' who confirmed the existence of the compound PbO . Sb203 as well as the form of the diagram. A disagreement was noticed, however, in that their liquidus temperatures over nearly the entire composition range were higher than those reported by Maier and Hincke. Barthel~ and pelze14 redetermined the liquidus curve at the PbO-rich end of the PbO-Sb@, system and agreed very closely with the results of Maier and Hincke. None of the investigators mentioned above reported any mutual solid solubility in the PbO-SbD3 system. Zunkel and Larson5 have determined the phase diagram for the PbO-rich end of the PbO-Sb203 system by slag-metal equilibrium studies in the Pb-PbO-Sb203 system and by thermal analysis studies in the PbO-Sbz03 system. A maximum solid solubility of 5.6 mol pct Sb203 in PbO was observed at the eutectic temperature of 604°C. Their results for the phase diagram agree favorably with those of Maier and Hincke. The vapor pressure of Sb2O3 in the temperature range from 470" to 800°C has been determined by Hincke, using a modification of the transportation meth~d.~ His results for temperatures below the melting point of Sba3 are the only data reported in the published literature. The predominant vapor species has been shown to be Sb,06 by Norman and staley.? Myzenkov and Klushin,8 using the boiling-point method, have determined the pressure of Sb406 above liquid SbD3 in the temperature range from 715" to 1025°C. The agreement between these two studies is not very close. A portion of the discrepancy lies in the fact that Hincke used silica crucibles, which were attacked by the liquid Sbz03 at high temperatures. This fact does not account, however. for the large difference observed at the melting point. ~aier' gives a brief summary of vapor pressure data for Sb,O, above pure liquid Sbz03 which agree quite well with the data of Myzenkov and Klushin at temperatures near the melting point. This paper describes the determination of Sb2O3 activity data in the PbO-Sb203 and Pb0-Si02-Sb203 (PbO/SiOz = 2) systems by the inert-gas saturation method. These activity data are compared with the data calculated by Zunkel and arson. EXPERIMENTAL Materials. The materials used in this investigation were analytical reagent-grade PbO (99.8 pct PbO, 0.14 pct insoluble in CHsCOOH, 0.02 pct not precipitated by HB, 0.1 pct CaO, and 0.08 pct SiOz), Sbf13 (99.6 pct Sb203, 0.004 PC~ C1-, 0.005 PC~ SO;-, 0.15 p~t AS, 0.001 pct Fe, and 0.03 pct other heavy metals such as Pb), and SiOz (chromatographic grade). Apparatus for Vapor Pressure Determinations. The apparatus used in this investigation consisted of a transportation reaction system with two separate gas trains. The argon transporting gas was first mixed with a small amount of hydrogen, metered, and dried by passage through silica gel and anhydrone drying tubes arranged in series. After this preliminary drying, the argon was passed through copper wool at 500°C to convert the residual oxygen to water vapor which was removed by three anhydrone drying tubes. A second stream of argon was metered and dried and then passed around the outside of the alumina reaction tube to flush away the volatile species to pre-

Jan 1, 1970

By Norman Goss

IT is generally agreed that cold-working mechanically refines the grains into smaller fragments and with continued working these are oriented with certain crystallographic directions bearing a relation to the direction in which the metal is worked. Some of the energy expended on the metal during plastic deformation appears in the form of heat, but a very small portion remains in the metal as stored energy. The entropy, specific heat capacity, temperature at which recrystallization will just begin, density, ductility, elasticity, tensile strength, and resistance to corrosion are affected. These properties have been studied extensively and some of the changes in the physical properties due to cold-working were attributed to lattice distortion.1-8 The broadening of the K. lines on the X-ray diffraction diagrams of plastically deformed metals is believed to indicate lattice distortion, and consequently the existence of internal stresses. The evidence supporting this theory rests solely upon the observed experimental fact that the dif-fraction lines are broadened and the K a doublets are completely diffused. Elam9 has reviewed the matter of lattice distortion in relationship to the hardening of metals by plastic deformation. The X-ray diagrams of plastically deformed metals differ in general from annealed metals. The hardening of a metal was believed due to lattice distortion.9 The resolu-tion of the doublet is lost when a metal is cold-worked and the Lane spots are elongated. At one time this elongation was thought to indicate the elastic bending of the crystal planes. However, more careful work showed that the asterism was due to new orientations developed within the fragmented grains during plastic deformation. Some theories attrib-uted the hardening to fragmentation of the grains into smaller units.

Jan 1, 1940

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 L. S. McNickle

Commonly accepted maintenance methods are being outdated by the rapid acceptance and use of more complicated hydraulic circuitry on modern mining equipment. It is no longer adequate to use the maintenance program to merely repair or sustain equipment operation. Ever increasing operating costs place a huge premium on lost production time. It has, therefore, placed the maintenance programs in the position of being required to alleviate equipment malfunctions on production shifts and still attain the maximum unit life from each component part. Ireland mine of Hanna Coal Co., which operates two production shifts and one maintenance shift per day, performs hydraulic maintenance with a plan that is geared to assure the bulk of work being handled on the midnight or maintenance shift. Production is thus allowed to continue without interruption from major hydraulic component malfunction. The plan is called selective maintenance because the specific part to be worked on and the time the work is to be accomplished are selected according to a definite plan.

Jan 10, 1961

By Sanford S. Cole

LABORATORY TESTS Takakuwa and Takamori' have applied the principle of phase inversion, well known in the chemistry of colloids, as a means of evaluating the wettability of minerals and to classify some frothing agents. By determining the angle of contact across the liquid phase of an emulsion, it has been possible to readily determine the wettability of a mineral. When this angle is less than 90°, the emulsion is of the oil-water type, and if it is greater than 90a, then the emulsion is of the water-oil type. The authors replaced oil with benzene in their recommended operation. They studied this method with the influence of ethyl xanthene on galena, on activated or unactivated zinc blend and of sodium cyanide on chalcopyrite and zinc blend. Raffinot and Formanek" described a pilot flotation plant with a capacity of 33 to 66 lb per hr of ore which is at the Laboratory of the Sociktk Minerais et Metaux in Paris. The plant will handle about 440 lb of ore per 8-hr shift and a regular series of tests can be undertaken with two to three tons of ore. Ore is ground to 0.1 in. and blended in advance. The plant includes two mills used either as rod mills or ball mills, conditioners, four groups of three cells for rougher circuits, eight cleaner cells and two small mills for regrinding middlings. Automatic controls for the pulp level in the cells, automatic sampling and addition of flotation reagents by electric valves facilitate plant operation and help to produce regular runs in spite of small throughputs.

Jan 8, 1963

Ore deposits are commonly divided into two classes, syngenetic and epigenetic, according to whether the ore was deposited together with the enclosing rock or was introduced after its deposition or solidification. Epigenetic deposits, which are by far the more important class, owe their formation to the channels that permitted the ingress of their metals, and both classes are, subject to great modification by post-mineral changes in the containing rocks. A discussion of the structural features of rocks, therefore, necessarily precedes any consideration of ore deposits or processes of ore deposition. The arrangement of sediments in parallel and approximately horizontal layers is called stratification, and is an original property of sedimentary rocks. Successive strata of the same sedimentary bed commonly differ from each other in some minor characteristic, such as texture or color, which results in a bedded or stratified appearance. The subjection of a rock to pressure develops within it parallel planes of weakness, called cleavage planes, along which the rock breaks into relatively regular slabs or blocks; the direction of these cleavage planes, which bear no relation to stratification, is determined by the direction of the pressure that produced them. Where there are more than one set of cleavage planes, one of them is likely to be more prominent than the others. In sedimentary rocks, the cleavage may coincide with the stratification but more commonly cuts across it. Van Hise has defined cleavage as the "capacity present in some rocks to break in some directions more easily than in others." Cleavage, therefore, does not imply the existence of subdivisions, but rather the tendency to subdivide along certain planes.

Jan 1, 1932

By Robert S. Williams

On several occasions, when 60-40 brass is first obtained in the beta condition by quenching at about 825" C. and is then reheated, the writers have noticed that reerystallization will take place in the form of twin crystals at the grain boundaries of the original beta crystals. It was, therefore, thought that interesting results would be obtained if this twinning process was studied further, especially as to the temperature at which it first occurs. The material used in the investigation was a bar of extruded muntz metal, 1/2 in. in diameter, and of the following composition: Copper, 60.21 per cent.; zinc, 39.73 per cent.; lead, trace; iron, trace; tin, nil. Specimens 1 in. in length were sawed from this bar and a hole was drilled into the side of each specimen until it reached the center, and the tip of a platinum-platinum rhodium thermocouple was inserted. A small Hoskins' resistance-type electric furnace was used for heating the specimens. The specimens were first heated at 840' C. for 2 hr. and then quenched ' in cold water, in order to get the material entirely in the beta state. In every case, in the reheating process, the furnace was brought to the desired temperature before the specimen was introduced. The time occupied in preheating was from 20 to 30 min. By sawing back 1/4 in. on each side of the hole, two parts were obtained from each specimen and duplicate observations were possible. The specimens were held at the reheating temperatures for periods of 15 min., 30 min., 1, 2, and 4 hr. All specimens were etched with a freshly prepared mixture of equal volumes of concentrated NH4IOH and H2O2.

Jan 1, 1924

By William Priestley

IN THE manufacture of gun forgings and other steel parts that, in service, are subject to sudden high stresses and shocks, it is most desirable to use steel possessing the greatest toughness and ductility possible without sacrifice of strength. In order to obtain this condition, it is necessary to procure steel that shows the highest possible elongation and reduction of area without lowering the tensile strength and elastic limit. Proper heat treatment of the steel can control this condition within certain limits. When heat treatment has failed to produce the desired results, metallurgists have used steels containing molybdenum, zirconium, vanadium, chromium, tungsten, etc. The purpose of this paper is to describe a method by which these desired physical properties may be procured-by the elimination of certain impurities that inherently exist in steel made by the open-hearth process, and without the use of expensive alloys. DESIGN OF GUN FORGINGS In the manufacture of gun forgings, a certain elastic limit is fixed by the designer, and the walls of the gun are made of the proper thickness, allowing a suitable factor of safety for the high stresses and sudden shocks that occur during gun firing. The elastic strength of the gun is about 1.4 times the stress set up at any point along the bore of the gun during firing with the maximum powder charge.

Jan 12, 1921

By W. D. B. Motter

DURING the early development of blasting with liquid oxygen explosives the trend of experimentation was towards increasing the effectiveness of the explosive. Its characteristic of becoming inert after evaporation of the oxygen content made a strong appeal from the standpoint of safety, especially with missed holes. It later became apparent, however, with practical use of this explosive, that LOX lacked certain other safety characteristics. As its effectiveness was increased, it became more subject to detonation by impact. The object of this paper is to show the steps taken by one operating company to achieve greater safety in the large-scale handling of liquid oxygen explosives.

Jan 1, 1933

By Amos P. Brown

PYRITE, the bisulphide of iron, FeS2, is found more or less in all coal-beds: but, as a rule, in certain definite forms. More than any other impurity, it detracts from the commercial value of a coal-deposit, and yet its presence is so universal that it might almost be said that there is no coal entirely free from pyrite. My observation has been confined to the Pennsylvania bituminous and semi-bituminous coals, and to them, therefore, my remarks will be confined. Certain generalizations which I may make, however, will be found of universsl application. The lowest members of the coal-formation, No. XIII. of the Pennsylvania bituminous region, are nearly always pyritiferous, and in many cases highly so. In Cambria county, for instance, coalbed A, the Brookville, is locally known as the " Sulphur seam." The Lower Kittanning, in parts of Clearfield county, is so sulphury as to be almost unmarketable, though otherwise it is a strong locomohive coal. In Mercer county the Pardoe bed, so extensively mined there, carries great quantities of sulphur in the form of pyrite, though usually this can be separated in such a way as to detract little from the market-value of the coal. The other coal-beds of the Lower

Jan 1, 1888

For many years the occurrence of gold in the Coeur d'A1ène region had been rumored among the pioneers of the Northwest. It is stated that as early as 1853 gold was discovered in this district by Donelson, of the Stevens expedition, but the hostility of the Indians prevented prospecting. In 1858, when Lieutenant John Mullan surveyed the military road across the Bitter hot mountains, the members of his expedition, most of whom had mined in California, noticed sundry outcrops of good-looking quartz, and some of them actually found gold, as is recorded in a letter that Mullan wrote, from Washington, in 1884. The first successful prospector in the Coeur d' Alène was Tom Irwin, who worked a quartz vein on the Mullan road in the spring of 1879. Two years later he met A. J. Prichard, who was engaged in the lumber business; he told him what he thought of the chances of placer mining in the upper reaches of the Coeur d7AlBne river. This was in 1881. Prichard became keenly interested, and himself found gold on several creeks, one of which is now known by his name, at a place close to the site of the town of Murray.* In 1883 Prichard located a number of claims, and shortly afterward he wrote a letter to the members of a Liberal League to which he belonged, inviting them to "secure the lion's share" of the mineral wealth he had uncovered. His letters caused a stampede from Montana and Colorado, and from South Dakota also, to the Coeur d'Alène gold belt in the summer of 1883. A town, named Eagle City, was surveyed; in 1884 lots sold at prices ranging from $200 to $2000. The buildings were made of logs and shingles. Shoveling of the snow in' front left s

Jan 1, 1932

By W. J. Millard

VAGUE rumors and stories have been heard, from time to time, about the diamond and gold deposits of southern Venezuela. It is perhaps appropriate, at this time of revived interest in gold mining, to publish a few facts in regard to this country, which has been undergoing exploration since the fifteenth century. Gold and diamonds are found principally in the State of Bolivar which lies in southeastern Venezuela and is bounded by British Guiana on the east and Brazil on the south (see Fig. 1). The famous Mt. Roraima is situated at a point where these three countries meet in a common point (see Fig. 2). Some gold is also found in the southern part of the territory of Amacuro. Good oil prospects exist in the northern part of this same territory. Diamonds are found on the Caroni river from Rio Paragua to the village of Guri. Another small district is on the headwaters of the Cuyuni river. Quartz veins containing gold are chiefly exploited in

Jan 1, 1931

By R. C. Weed

LEACHING in place at Cananea began in the 1920's on a limited scale. The first plants were small wooden boxes located underground in the Capote and Oversight mines, and output was low. Scrap iron was used as precipitant. Later several other small plants were started up. Leaching was limited entirely to underground areas, and production remained low. The Veta precipitating plant, the first on a larger scale, was put into operation in the late 1920's. After a period of intermittent service it was rebuilt in 1946 and has since been running continuously. In 1943 work on the Colorada open pit was started. This produced 40 million tons of waste, which averaged 0.20 pct capper. When these dumps had aged a few years it was decided to leach them on a large scale, and after considerable research and investigation a leaching system of pumps and pipelines was laid out and installed. At the same time the Ron-quillo precipitation plant was built to treat the copper solutions from the pit dumps. This plant started operation in March 1953. Leaching areas consist of the Colorada pit dumps and various mined out and caved underground stopes. The principal mineral, chalcocite, leaches readily in a weak sulfuric acid solution containing ferric iron. Enough pyrite is contained in the areas to produce an acid-ferric iron solution strong enough to dissolve the copper. Each area is studied to determine the best method of distributing the water over it and the best method of collecting the copper-bearing solutions after leaching has taken place. Water is generally distributed by means of ponds, ditches, and sprays. Spraying has proved the best method of spreading the water evenly; however, in a dry climate some water is lost through evaporation. After passing through the leachable material the solution is collected underground by dams and bulkheads and on surface by dams. An effort is made to give the maximum storage capacity practicable.

Jan 1, 1957

By C. S. Duncan, S. Scuro, D. R. Muss

Work is vepurted which was aimed at accentuating the pec14liar attributes of the GaAs laser diode, namely its sutzull size and its high efficiency. This has been done by reducing- transport losses in the bulk p and n regions of the diode and combining many of. these diodes into series stacks with common optical cazlities. The result of this effort is a nearly monochromati source at about 8450A With a luminous areu 0.05 by The GaAs laser diode is an attractive pulsed light source in the near ir because of its ability to emit very large pulse powers and its small size. In addition to this, the device is efficient; and the higher the 0.05 cm emitting peak pulse po we rs at greater than 300 LC at repetition rates below 200 pps into a cone about 0.01 steradians when operated at 77°K. The results of nzeasuvetnents of peak optical power and spectra frorr~ these stacks are reported and some conclusions are drawn about the vole the individual diodes play in the stacked operation. peak output power, the more efficient it is. The limit for the amount of power that these diodes can emit is the transient and average dissipation associated with the pumping pulse. This power dissipation arises primarily from transport across the bulk regions of the diode; this fact, along with the relatively low thermal conductivity of the GaAs, led us to the conclusion that higher power

Jan 1, 1968

By Mark A. Ammon

The two most widely used methods of measuring hardness are the Brinell and the scleroscope. In the Brinell method a hardened steel ball is pressed into the steel under a definite load and the area of the resulting depression is measured. The load in kg. per sq. mm. of the area of the depression is taken as a measure of the hardness. Within certain limits the hardness number so determined is independent of the load or the size of the ball. In the scleroscope method a small weight carrying a diamond point is dropped through a glass tube upon the steel and the amount of rebound is taken as proportional to the hard-' ness. In both methods the scale of hardness is an arbitrary one; however, they agree in a comparative may, that is, a steel showing 50 per cent. increase in hardness by the Brinell test mill show approximately 50 per cent. increase in hardness by the scleroscope test. Yet upon consideration of the two methods it appears that, upon a steel which has been carbonized, this should not be the case ; for the scleroscope method gives almost exclusively the surface-hardness, and the condition of the material below the surface has but a slight bearing upon the hardness number. The results given by the Brinell method should, however, be the exact opposite; for the depth of penetration 'of a ball pressed into the steel would be dependent to a large extent upon the condition of the material below the surface. This is particularly obvious when it is considered that the size of the ball ordinarily used in the Brinell method is 1 cm. (about 8 in.) in diameter under a load of 3,000 kg., while the diamond point of the scleroscope is in the neighborhood of 0.01 in. across, fitted in a hammer of about 0.5 oz. weight and dropping from a height of 10 inches.

Jan 1, 1913

By Frederick Laist

THE past year has witnessed no radical changes in methods for the reduction and refining of copper. The Carson litigation was finally brought to a close ant1 the copper smelter is again free to introduce charge into his reverberatory furnaces in whatever manner suits him best. This litigation naturally led to much experimentation with various methods of charging and with various types of bath. In some cases the charge was introduced more or less centrally on a relatively dry hearth and in other cases into a bath of greater or less depth. The results of these furnaces were meticulously compared with the results obtained in side-charger furnaces, and it was apparent that it made little, if any difference how a given furnace \\.as charged so long as care was taken that there was always something in the furnace for the flames to work on. So long as this requirement was complied with, consumption of fuel per ton of charge smelted and tonnage smelted per furnace day remained substantially the same regardless of the method of charging or the depth of bath employed. In some instances the center-charged deep-bath furnaces gave slightly better results than the side-charged particularly with respect to copper losses. The slags of the deep-bath furnaces are generally a little cleaner

Jan 1, 1930

By Blamey Stevens

(Butte Meeting, August, 1913.) THE following paper aims to make a full explanation of the phenomena of rock jointing: It may be unnecessary to give any general description of what are termed joints in rocks, but Professor Geikie's clear and faithful generalizations are so illuminating that no excuse need be given. for introducing the following and other quotations into this paper "Almost all rocks are traversed by vertical or highly inclined divisional planes termed joints. These have been regarded as due in some way to contraction during consolidation (fissures of retreat) ; and this is no doubt their origin in innumerable cases. But, on the other hand, their frequent regularity and persistence across materials of very varying texture suggest rather the effects of internal pressure and movement within the crust." 1 General Explanation.-In this paper I show that the phenomenon of jointing may to a large extent be accounted for by the pressure of the water contained in the pores of the rock. To understand this, each constituent grain of the porous material may be considered to be separately compressed by the water which submerges it. As all the grains are held together by cohesion, the whole mass is contracted by this pressure. In an indefinitely extended mass, however, there must be a limit to the possible contraction without rupture, because the material is restrained from moving freely by other material around its boundaries. The mass of rock thus becomes broken up. This phenomenon is known as '" shrinkage " jointing. The term " shrinkage " is an apt one, if it be understood that the shrinkage of the rock is often brought about by change of stress. Stresses.-The compressive component of water stress on the individual grains is evidently the same as that of the water with which it is in contact. This is so, both before and after the jointing is formed. Before the jointing is formed there is, however, a tensile stress in one or more directions which keeps the material from contracting. .

Jan 7, 1913

By Marcus Grossmann

THIS paper offers for consideration certain somewhat radical modifications in the iron-carbon diagram, these modifications being the result of the presence of notable amounts of alloying elements. When only small amounts of alloys are present, 'the standard iron-carbon diagram (Fig. 1) can be used with but insignificant changes; when larger amounts of Chromium, Per Cent FIG. 1.-IRON-CARBON DIAGRAM. FIG. 2.-IRON-CHROMIUM DIAGRAM. alloys are present, however, it assumes a distinctly altered appearance. No comment is offered for the present except to call attention to the delta area, A4BM, which represents a region of mixtures of austenite and delta iron, just as area A3SP represents mixtures of austenite and alpha iron.

Jan 12, 1926

By C. F. Cornell, R. C. Emmett, D. A. Dahlstrom

FOR many years the disk-type and cloth-covered drum filters have found widest application in liquid-solids separation, which uses continuous filters. The disk type is less expensive, occupies less floor space per square foot of filtration area, and re- quires negligible down time for filter media changing. However, because filter cloth is billowed out by the blowback in the cake discharge, it is very short-lived if the scraper blades are set too close. Consequently cake weight is very important in assisting cake discharge, which normally necessitates a minimum cake thickness of 3/8 to ½ in. Also, the vertical position of the disks eliminates the possibility of efficient cake washing for removal of soluble values. The disk-type filter is generally limited, therefore, to applications that require no cake washing and form relatively thick cakes within the normal range of filter cycle times. The conventional cloth-covered drum filter is a more flexible unit, permitting wider variation in the percentage of cycle time devoted to cake formation, dewatering, or washing, as required by the application. Thinner filter cakes can be discharged be- cause a horizontal line across the filter medium at the location of the scraper blade is equidistant from the edge of the blade at all points. The scraper blade therefore may be set a short distance from the filter medium or, where wire winding is not used, a floating scraper can be utilized so that the contour of the cloth can be followed. The drum filter is generally employed when there are difficult filtering slurries with resultant thin cakes or when cake washing to recover soluble values must be practiced.

Jan 2, 1958

By C. Altstetter

THE work herein reported is restricted to the carbides which occur in quenched and tempered AISI 43XX steels with carbon contents up to 0.40 pct and silicon additions of up to 3 pct. In view of the instability and extremely small size of the carbides formed at low tempering temperatures, the technique for successfully preparing specimens for X-ray diffraction will be outlined. The alloys listed in Table I were obtained through the courtesy of the United States Steel Corp. in the form of 1/2-in. rounds forged from 100 lb. induction furnace heats (except for 4337 which was a commercial heat). The stock was normalized and then swaged and drawn to 15 mil wire with anneals at 1200F between passes. The wire was austenitized for 45 min in evacuated vycor capsules and quenched into iced brine with simultaneous smashing of the capsule. Tempering was done in air with a water quench after tempering. The carbides were extracted in a simple cell using a solution of 1M KC1 and 0.5 pct citric acid with an initial current density of 0.1 amp per sq cm. One end of a short length of wire was immersed in the solution, and the current at constant voltage was noted as a function of time. After about an hour the current dropped sharply because of the decrease in specimen cross-section. At this point it was found that the dissolution could be stopped and that the very fine wire which then resulted was just large enough to permit handling of the extracted precipitate still clinging to it, yet so small that it diffracted and absorbed only a negligible amount of the X-radiation. This rod of residue with a convenient handle of undissolved wire was rinsed in distilled water. alcohol, and acetone. Then it was dipped in a thin solution of cellulose-acetate cement and dried in vacuum. The resulting specimen was straight, uniform in density, easily handled, but most important, was completely sealed and never exposed to air. Furthermore, the residue had never been subjected to strong acids or rough handling such as in the extraction-replica technique or in the complete extraction to a powdered residue. It was found that improperly coated specimens were pyrophoric, turning to oxide with a dull red glow as they were exposed to air and yielding patterns of Fe2O3 and Fe3O4. The steels containing 3 pct Si were especially difficult to prepare for this reason. The specimens were put in a 57 mm Straumanis camera with double pinholes or slits and irradiated with filtered-chromium radiation. Readable patterns were obtained in less than an hour. A preliminary finding of some note was that for both tempered and as-quenched specimens of steels 4337 and 4337 (1.5 Si). M23C6 patterns were found along with the patterns of other constituents of the residues. This result was somewhat surprising in that previous investigators had reported that this carbide did not appear in a 0.38 pct C, 0.48 pct Mo steel1 or in chromium steels of less than about 10 pct Cr.2 Although the total amount of carbide-forming alloying elements is less than 2 pct, due to their mutual interaction and the action of the plastic deformation in promoting equilibrium, this carbide was able to form even in the steel containing 1.5 pct Si. M23C6 was not detected in the 4337 (3.0 Si) steel and the lower-carbon steels were not investigated in this condition. It is very likely then that the steels studied herein underwent a fourth stage of tempering during the anneals at 1200°F. This result has significance in that even a small amount of undissolved M23C6 in a low-carbon, low-alloy steel would exert a large effect on its hardenability. Its presence would also influence the mechanical properties by decreasing the carbon content of the matrix. Annealing in vacuum for 1 to 4 hr in the austenite field removed all traces of MZ3C+ The results on carbide precipitation during tempering, summarized in Table I, are in agreement with those of Klingler et al.3 for the higher carbon steels. For the AISI 4337 steels it is noteworthy that in the steels with added silicon the E carbide persists to longer times and higher temperatures and that silicon delays the formation of cementite. The results for the lowzr-carbon steels parallel those of the higher-carbon grade. The appearance of E carbide in the AISI 4315 is significant. There is considerable disagreem-nt in the literature as to whether this carbide forms in the tempering of steels containing less than about 0.2 pct C. Following the detection of E carbide in a 0.18 pct C plain-carbon steel,4 its occurrence in a steel containing chromium and molybdenum should be expected. The fact that the low-carbon steels have the same carbide-precipitation sequence as the high-carbon steels has bearing on the larger problem of the exact tempering reactions in all steels. Following the suggestion of Roberts et al.,' the first stage has been generally assumed to result in a metastable equilibrium of c carbide and martensite of about 0.25 pct C. From this it was concluded that a steel having less than 0.25 pct C should then be under-saturated with respect to c carbide and should not precipitate this carbide upon tempering. In view of the experimental findings of c carbide in steels hav-

Jan 1, 1962