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By Robert M. Keeney

Important recent developments in the melting and annealing of non-ferrous metals include: 1. Melting of nickel silver in the vertical ring induction furnace. 2. Electric melting of stereotype metal. 3. The rotary-drum gas-fired brass melting furnace. 4. The low-frequency coreless induction furnace. 5. Finishing annealing of brass sheets with city gas1 replacing wood in the large brass-rolling mill. 6. Electric annealing of brass and copper tubing and sheets. 7. Replacement of oil by gas and electricity in the annealing of nickel-silver shells and stampings. Melting Nickel Silver in Vertical Ring Induction Furnace Although over 90 per cent. of the output of the brass rolling mills in the United States is now melted in electric furnaces,2 until recently a considerable part of the output of nickel silver has been the product of the pit fire. The application of the electric furnace to the melting of nickel silver has been slow for several reasons: (I) Until recently no lining has been available that gave a satisfactory life in the vertical ring induction furnace when melting nickel silver; (2) the rocking arc furnace so widely used in the foundry does not appear to have been favored by the rolling mill for melting nickel silver, possibly because the gases present may affect the quality of the alloy; and (3) the exclusive rights to the use of the high-frequency coreless induction furnace (which has proved very satisfactory for melting nickel silver) for the wrought brass industry are controlled by one concern. A little over one year ago the first vertical ring induction furnace to be used for melting nickel silver in the Naugatuck Valley was placed in operation. This was followed by two more in the same mill, and by

Jan 1, 1930

By Walter Crafts

Structural steels containing chromium have become widely used in the last 20 years. In the earlier part of this period the major applications were in chromium-molybdenum aircraft tubing and similar special high-strength steels. During the past 10 years there has been a notable expansion in the use of chromium-bearing steel for structural purposes when welding was utilized for fabrication. The chromium-bearing steels introduced by Saklatwallal (chromium-copper), Kinzel2 (chromium-manganese-silicon), and Schultz3 (chromium-copper) are being extensively used at the present time. General Effects of Chromium Chromium is so widely known for its carbide-forming tendency that its capacity to stabilize oxygen, nitrogen, and phosphorus is often overlooked. In low-carbon steels of the structural type these so-called secondary characteristics become more prominent. For this reason also, chromium in structural steel is definitely a toughening agent. As the carbon content is increased, the more widely known hardening effect becomes more evident. In low-carbon steels chromium increases the notched-bar impact strength substantially. This property persists at subzero temperatures and is utilized for low-temperature service in chromium-copper steel.4 Chromium also reduces any tendency to strain-aging embrittlement. In addition to improving the toughness of steels with the usual impurities, chromium has the specific property of counteracting the brittleness induced by high phosphorus.5,6 In steels low in carbon and alloys, chromium has an almost negligible effect on tensile strength, and a hardening influence is noticeable only in the stronger steels. The ductility of welds adjacent to the base plate is also improved by chromium, both in the range of foolproof welding steels having strengths of less than 80,000 lb. per sq. in. as well as in the higher strength steels.

Jan 1, 1939

By Eric Jette

THE unusual physical, electrical and magnetic properties of the iron-nickel alloys has given rise to a voluminous literature. This work will be reviewed critically in "The Alloys of Iron and Nickel," a monograph of the Alloys of Iron Research Series, soon to be published. In what follows we shall therefore confine ourselves to those of the earlier investi-gations that involved the use of X-ray crystal-structure methods. The earliest X-ray work on the iron-nickel system was by Miss Andrews1. Using the powder method of X-ray analysis purely as a means of identifying the phases present, she located a region between 20 and 30 weight per cent nickel in which body-centered and face-centered phases coexisted. No lattice constants nor details of heat-treat-ment were reported. Bain2 also reported some qualitative observations. McKeehan3 made a systematic investigation over the whole of the system, giving many of his alloys four and some five different heat-treatments. In alloys furnace-cooled from 900° to 950° C. he found two coexisting phases between 0.15 and 30 per cent nickel. The precision of the lattice-constant measurements was low in comparison with what can be obtained today.. Even for alloys of the same heat-treatment, differences in the constants were often between two and ten parts per thousand. In regions where no change of lattice constant with heat-treatment should occur, differences of the same order of magnitude were found. Since the maximum change in the lattice constant of nickel with change of composition is only about 2 per cent of the constant for pure nickel, these variations in the constants for a given alloy cause the points

Jan 1, 1936

By H. E. McKinstry

MOVEMENT on a fracture of irregular shape can cause local widening of the fissure and thereby offer freer channelways for circulation of ore-depositing solutions. This influence, coupled with large areas of wall rock available for reacting with ore solutions in brecciated and shattered ground can account for locally active deposition of metals and the resulting ore shoots. Such irregularities in the fracture system may be caused by local variations in the strength of rocks and by pre-existing lines of weakness, especially if these stand at favorable angles to certain components of the fracturing stress. Therefore correct interpretation of the mechanics of fracturing should permit deductions as to structurally favorable places on unexplored portions of the vein system. INTRODUCTION IT has long been recognized that movement on a curved or irregular fault surface is capable of separating the walls in certain portions of the fault, but until very recent years the importance of this mechanism as a factor in localizing ore shoots has escaped proper recognition. A short time ago W. H. Newhouse' presented a careful analytical study of displacements and their corresponding open spaces. For reasons that will be discussed later, it frequently happens that portions of the vein which are favorably oriented are not merely wider but also richer than the average. In many cases the widening with its accompanying richness coincides with very minor changes in the dip or strike of the vein, irregularities that commonly escape notice unless the vein is mapped in detail and a careful geometrical analysis made. While the relationship between the width of the vein and the changes in dip or strike has been recognized as a matter of observation, the irregularities have been accepted as more or less the result of accident. There has been very little effort except in isolated cases to find out the causes of these changes in dip or strike. Yet it is clear that if the causes can be recognized and expressed in terms of geologic structure the geologist will know where to look for repetitions of these favorable conditions either on extensions of the same vein or on adjoining veins. Any lack of understanding of the causes is due to the limitations of our ability to interpret our observations and not to the sheer capriciousness of

Jan 1, 1941

By A. C. Bulnes

This paper applies the methods of statistical analysis to the interpretation of core analysis data of dolomitic limestone from the San Andres formation at Wasson and the Clearfork formation at Fullerton. Probability relationships are shown to connect the porosity and the permeability and the porosity and the fluid saturation. For example, the porosity-permeability relationship expresses the probability that a sample of porosity,f, will or will not be permeable. The over-all porosity frequency distribution of the reservoir together with the frequency curves of permeability (one for each class interval of porosity) provide a precise basis for computing the weighted average productive porosity of the reservoir for any assigned value of the minimum productive permeability. The probability that the permeability of a core specimen from Fullerton will exceed a given value appears to be dependent on the percentage porosity of the specimen, its void structure type (i.e., porosity in the qualitative sense), and the given value of the permeability. If continuous profiles of void structure type and porosity are available together with the appropriate porosity-probability of permability plots, the nes pay thickness may be estimated. The Invasion Index of a well is defined in terms of the porosity and permeability data. This index is suggested as a basis for comparing wells as regards their suitability as fluid-injection wells. Three problems of importance in the exploitation of limestone reservoirs may be stated as follows: 1. The determination of the productive porosity of the reservoir. The productive porosity is defined as f = fPVP/V [II in which Vp, is the volume of the reservoir that is sufficiently permeable to oil to give up an appreciable fraction of its original oil in place during the economic life of the reservoir; fp, is the arithmetic mean porosity of the permeable volume v*, and V is the total volume of the reservoir. 2. The determination of the number of feet of oil-bearing porous rock that will produce at a commercial rate into the well bore; i.e., the net pay thickness. 3. The choice of fluid-injection wells in a secondary recovery program. The ultimate recovery of the reservoir is proportiona1 to the productive porosity. The productive capacity of the well is proportional to the net pay thickness. The principal purpose of this paper is to show that the methods of statistical analysis when applied to core analysis data of dolomitic limestones offer a useful approach to the solution of these three problems, as well as others of importance in reservoir engineering. The use of these methods was suggested by the work of Jan Law.1

Jan 1, 1946

By A. C. Bulnes

This paper applies the methods of statistical analysis to the interpretation of core analysis data of dolomitic limestone from the San Andres formation at Wasson and the Clearfork formation at Fullerton. Probability relationships are shown to connect the porosity and the permeability and the porosity and the fluid saturation. For example, the porosity-permeability relationship expresses the probability that a sample of porosity,f, will or will not be permeable. The over-all porosity frequency distribution of the reservoir together with the frequency curves of permeability (one for each class interval of porosity) provide a precise basis for computing the weighted average productive porosity of the reservoir for any assigned value of the minimum productive permeability. The probability that the permeability of a core specimen from Fullerton will exceed a given value appears to be dependent on the percentage porosity of the specimen, its void structure type (i.e., porosity in the qualitative sense), and the given value of the permeability. If continuous profiles of void structure type and porosity are available together with the appropriate porosity-probability of permability plots, the nes pay thickness may be estimated. The Invasion Index of a well is defined in terms of the porosity and permeability data. This index is suggested as a basis for comparing wells as regards their suitability as fluid-injection wells. Three problems of importance in the exploitation of limestone reservoirs may be stated as follows: 1. The determination of the productive porosity of the reservoir. The productive porosity is defined as f = fPVP/V [II in which Vp, is the volume of the reservoir that is sufficiently permeable to oil to give up an appreciable fraction of its original oil in place during the economic life of the reservoir; fp, is the arithmetic mean porosity of the permeable volume v*, and V is the total volume of the reservoir. 2. The determination of the number of feet of oil-bearing porous rock that will produce at a commercial rate into the well bore; i.e., the net pay thickness. 3. The choice of fluid-injection wells in a secondary recovery program. The ultimate recovery of the reservoir is proportiona1 to the productive porosity. The productive capacity of the well is proportional to the net pay thickness. The principal purpose of this paper is to show that the methods of statistical analysis when applied to core analysis data of dolomitic limestones offer a useful approach to the solution of these three problems, as well as others of importance in reservoir engineering. The use of these methods was suggested by the work of Jan Law.1

Jan 1, 1946

By H. F. A. Hergt, K. L. Sutherland, J. Rogers

In 1938 Ralston4 reviewed the many attempts to find a satisfactory collector for the separation of cassiterite from its ores and in 1944 Dean and Ambrose2 summarized some further attempts. Generally, soaps and amines are effective but nonselective collectors. We have discovered that reagents containing either the polar group — SO4- or — SO3- are excellent collectors for cassiterite and promise to be selective. The response to these reagents of cassiterite and of minerals commonly associated with it was studied, using the captive-bubble technique. Using these fundamental data, the practicability of separation and concentration of tin was investigated by flotation tests in a 2000-gram Denver cell. Experimental Methods Reagents All inorganic reagents were of Analar grade. The preparation and purification of sodium cetyl sulphate, cetyl trimethyl-ammonium bromide, laurylamine and cetylamine have been previously described.5 The other collectors were commercial surface-active agents, which were used without purification. Tests Captive-bubble Tests and Cylinder Flotation Tests have been previously de- scribed.5,10 The full lines shown in the figures relating solution composition to contact (flotation) distinguish solutions in which contact (flotation) is possible from those in which it is not. The curve is derived by successive approximation and the accuracy is ±0.2 pH units and ± 5 mg. per liter of collector or depressant. Solution compositions for which it was shown experimentally that contact or flotation is possible are marked by a circle, those for which it is not possible, by a cross, and those for which it is doubtful by a cross within a circle. It is assumed that at all other solution compositions within (without) the curve, contact or flotation is possible (not possible). After testing in the collector solution, the mineral was removed, washed, and tested by the captive-bubble method in water, or floated in a cylinder with frother only. In this way the composition of solutions in which a mineral was conditioned but in which properties of the collector solution prevented contact or flotation can be defined. The composition of solutions in which conditioning was possible lie between the full and broken curve, and the experimental results are indicated by a square. The curves show the limits of composition of solutions in which flotation in a cell would be possible but many factors other than those considered in these the determine recovery and grade of a given mineral in practice. Flotation Tests in 500 and 2000-gram Denver SUbmachines,—Melboume tap water, containing 12 parts calcium, 6 parts

Jan 1, 1947

By J. Rogers, H. F. A. Hergt, K. L. Sutherland

In 1938 Ralston4 reviewed the many attempts to find a satisfactory collector for the separation of cassiterite from its ores and in 1944 Dean and Ambrose2 summarized some further attempts. Generally, soaps and amines are effective but nonselective collectors. We have discovered that reagents containing either the polar group — SO4- or — SO3- are excellent collectors for cassiterite and promise to be selective. The response to these reagents of cassiterite and of minerals commonly associated with it was studied, using the captive-bubble technique. Using these fundamental data, the practicability of separation and concentration of tin was investigated by flotation tests in a 2000-gram Denver cell. Experimental Methods Reagents All inorganic reagents were of Analar grade. The preparation and purification of sodium cetyl sulphate, cetyl trimethyl-ammonium bromide, laurylamine and cetylamine have been previously described.5 The other collectors were commercial surface-active agents, which were used without purification. Tests Captive-bubble Tests and Cylinder Flotation Tests have been previously de- scribed.5,10 The full lines shown in the figures relating solution composition to contact (flotation) distinguish solutions in which contact (flotation) is possible from those in which it is not. The curve is derived by successive approximation and the accuracy is ±0.2 pH units and ± 5 mg. per liter of collector or depressant. Solution compositions for which it was shown experimentally that contact or flotation is possible are marked by a circle, those for which it is not possible, by a cross, and those for which it is doubtful by a cross within a circle. It is assumed that at all other solution compositions within (without) the curve, contact or flotation is possible (not possible). After testing in the collector solution, the mineral was removed, washed, and tested by the captive-bubble method in water, or floated in a cylinder with frother only. In this way the composition of solutions in which a mineral was conditioned but in which properties of the collector solution prevented contact or flotation can be defined. The composition of solutions in which conditioning was possible lie between the full and broken curve, and the experimental results are indicated by a square. The curves show the limits of composition of solutions in which flotation in a cell would be possible but many factors other than those considered in these the determine recovery and grade of a given mineral in practice. Flotation Tests in 500 and 2000-gram Denver SUbmachines,—Melboume tap water, containing 12 parts calcium, 6 parts

Jan 1, 1947

By M. S. Burton, G. V. Smith, A. Rosen

The kinetics of re crystallization and the effect of recovery on recrystallization of pure iron were investigated within the temperature range of 517" to 632 OC. Grain growth and activation energies were also studied. Two stages can be distinguished during recrystallization; the first is gvowth-controlled and the second is nucleation-controlled. The extent to which the first stage succeeds before the second stage begins depends on both temperature of recrystallization and temperature of recovery. The softening of cold-worked metals and alloys due to transformation of the deformed crystals to strain-free equiaxed grains during annealing is well-known, and early inestiators established that recrystallization kinetics is strongly influenced by minute quantities of impurities. Generally, it is believed that impurities decrease the rate of recrystallization and the rate of grain growth. To understand the basic phenomena of recrystallization, investigations should be on pure materials. Most of the research on high-purity materials has been on metals having the fee Bcc materials, and especially high-purity iron, have been studied only in recent years. It is known that recovery may influence recrystalliation;" however, no general description of the influence, applicable to all materials, has been presented. This paper presents results of a study of the recrystallization kinetics of high-purity iron, after 60 pct cold deformation by drawing, with particular reference to the influence of recovery on the rates of recrystallization and grain growth. From observations of these rates, conclusions are drawn concerning nucleation. MATERIAL AND EXPERIMENTAL PROCEDURE Preparation of Material. High-purity iron, prepared by zone refining of vacuum-melted electroiytic iron at Battelle Memorial Institute under sponsorship of the American Iron and Steel Institute, was used in this study. Table I gives the reported chemical analysis of the material, taken at a point near the last molten zone and thereby rep- resenting the maximum impurity level for the entire bar. Prismatic specimens, approximately 10 x 10 X 50 mm, were sawed from the 50-mm-diam bar, perpendicular to the zone-refining direction, and turned to cylindrical shape. These specimens were sealed in quartz capsules under vacuum, approximately 10"e mm Hg, austenitized at 930° C for 15 min, slowly cooled, removed from the capsules, and cold-worked in air by swaging to approximately 20-pct reduction of area. The encapsulating, austenitizing, and swaging operations were repeated two additional times, after which the samples were encapsulated, austenitized, and cold-drawn to 60-pct reduction of area. A further vacuum anneal at 630°C for 120 min and cold drawing to 60-pct reduction of area produced wire 2.8 mm in diameter. The drawn wire was electropolished to remove deformed material on the surface, after which it was sawed into 4-mm-long specimens for the recrystallization study. Microscopical examination before the final cold reduction revealed equiaxed grain structure with very fine grains in a thin layer near the surfaces of the specimen and nearly uniform ASTM 3-4 grain size in the center. Recrystallization Heat Treatment. a) Direct Recrystallization of Cold-Worked The 60 pct cold drawn iron specimens were recrystallized at five temperatures, 517, 556, 590°, 612, and 632C, in a lead bath covered with graphite (the temperature was controlled to 1°C). Specimens were treated for twelve different times at each temperature, and all were water-quenched after heat &eatment. b) Recrystallization Following Preliminary Recovery Heat Treatment. After cold working, specimens were sealed into quartz capsules under vacuum, 105 mm Hg, and recovery-annealed at 362", 400", and 440°C for 20 hr prior to recrystallization. No evidence of recrystallization was found

Jan 1, 1964

By T. L. Fritzlen

EXTRUSION of aluminum alloys in this country is performed mainly by direct extrusion, therefore this paper is confined only to factors affecting the rate of extrusion by this method. Many factors affect the rate of extrusion of aluminum alloys. It is the purpose of this paper to present a discussion on the factors that are subject to technical control. Most of them are closely related, so that a clear-cut distinction between them is rather difficult. However, an attempt will be made to evaluate the effect of each factor separately, as far as possible. The most important factors only will be considered, and these will be discussed in detail under three general headings: (I) characteristics of the equipment, (2) size and structure of the ingot, and (3) temperature of ingot, cylinder, and other parts. It is a well established fact' that the pressure and the speed of extrusion are related and are exponential functions of one another. Therefore, whenever a certain condition tends, for instance, to increase the pressure required for extrusion, it will reduce the extrusion speed if the pressure is maintained constant. For this reason, in this paper the effect of various conditions is expressed either in regard to their effect on the pressure required or the extrusion speed. Another established fact is the relationship between the temperature of the material being extruded and the pressure required to extrude. According to Schishokin,2 this relationship is of the exponential type, and as the temperature is increased the pressure required is decreased. It would seem from the preceding that the greatest rates of extrusion can be obtained by the use of higher temperatures. However, as is well known, other factors intervene to limit the rate of extrusion of aluminum alloys when increasing the temperature. These factors will be discussed in detail later. CHARACTERISTICS OF THE EQUIPMENT The capacity of the press determines the maximum unitary pressure that can be applied for any given cylinder diameter. Pressures used for extrusion of aluminum alloys range from approximately 50,000 lb. per sq. in. to 150,000 lb. per sq. in., dependent upon the alloy and the size of the shape extruded. Higher pressures could be used to advantage, but existing steels limit pressures employed in the production of extrusions. Numerous mechanical characteristics of the extrusion press affect extrusion rate. The most important characteristics of the press itself are: (I) sensitivity of the main pressure valve and accuracy of pressure gauges, (2) accuracy of equipment to heat the cylinder uniformly and to control cylinder temperature, and (3) accuracy of means of measuring the speed of extrusion. The variables subject to control during the extrusion operation are pressure, temperature, and speed, and it is evident that the preceding characteristics

Jan 1, 1945

By AIME AIME

AS director of Battelle Memorial Institute and as Chairman of the important O.P.M. advisory committee on metals and minerals, Clyde E. Williams numbers his acquaintances in the mineral industries by the thousands and h because his principal hobby is liking human beings, most of his acquaintancs are also his friends. Clyde is one of the many outstanding metallurgist, in the United States who started as a chemist. After graduating from the University of Utah in 1915 he was successively chemist for U.S. Smelting Refining and Mining Co., and at the Bureau of Mines station at Ithaca, N.Y. He then got into, metallurgical work and in 1920 he was appointed superintendent of the Northwest Station of the Bureau of Mines at, Seattle. Subsequently he was assistant to H. Foster Bain in metallugical work for the

Jan 1, 1942

By S. A. Mersol, C. T. Lynch, F. W. Vahldiek

The room-temperature Knoop hardness of single -crystal titanium diboride has been determined. Variations in microhardness have been correlated with orientation and structural imperfections in the crystals. Maximum differences in hardness values of 750 kg per sq mm with respect to orientation and 450 kg per sq mm with respect to substructure were found. The effects of etchants, load on indenter, and degvee of cracking of indentation were studied. The average hardness was determined as 2800 kg per sq mm on the as-grown crystals. Annealing increased the average hardness to 3375 kg per sq mm. ThE microhardness of polycrystalline titanium diboride approximating the stoichiometric composition TiB, has been studied by several investigators. The values for the Knoop hardness number range from 2710 kg per sq mm (Khn = 2710 kg per sq mm) to 3400 kg per sq mm.'-4 Samsonov et al.' reported a Vickers hardness number of 3400 kg per sq mm (Vhn = 3400 kg per sq mm) at 120-g loads for a 98 pct Ti + B material of 96 pct theoretical density. Recently Dunegan measured the Vickers hardness and obtained 2060 kg per sq mm with a 10-g load (Vhnlo = 2060 kg per sq mm), 1425 kg per sq mm for Vhnloo, and 1320 kg per sq mm for Vhnlooo. We have obtained a Khnloo = 3000 * 350 kg per sq mm for hot-pressed polycrystalline TiB2 that was 99.1 pct Ti + B and 96.6 pct of theoretical density. The present investigation has been made on single-crystal titanium diboride boules, and is believed to be the first such study on TiB, crystals of known orientation. EXPERIMENTAL The single crystals were prepared by a Verneuil-type process using an electric arc by the Linde Division of Union Carbide Corp. The largest specimens were 6 mm in diameter by 12 mm long. The crystals were of theoretical density (4.50 g per cm3) with a Ti + B content of 99.8 pct. The major impurities present were: 0.03 pct (by weight) 0, 0.06 pct C, 0.01 pct Si, 0.05 pct Fe, 0.01 pct Cr, and 0.01 pct Ni. The crystals were boron-rich, the average boron content being 31.S7 wt pct (stoichiometric value is 31.12 wt pct), and titanium-poor, the average titanium content being 68.2 wt pct (stoichiometric value is 68.88 wt pct). Titanium was determined gravimetrically by cupferron precipitation and boron by titration of H3B03 from a NaOH-fused specimen after removal of titanium with BaC03. The outer edge of the boule accounted for some of the excess boron. An electron-microprobe analysis showed that the titanium content increased from 60.0 wt pct at the edge to 68.5 wt pct at D, ~ 1000 p, where D, = distance from outer edge (see Fig. 5). X-ray measurements indicate that the boules are single crystals with considerable substructure. Upon etching this structure is seen in the form of a Widmanstatten-type rhombohedral line pattern in the basal (c) plane and a parallel "lines" pattern in the prism (a) planes. A typical WidmanstHtten-type pattern is seen in in Fig. 1. Electron microscopy reveals that the lines are less than 1 p across, which does not allow direct electron probe or microfocus X-ray determination of their composition. The identity of the second phase has not been established. It might be a higher boride or a nonstoichiometric TiB2. On annealing above 2200°C the precipitate is dispersed and dissolves in the matrix. The best etchants found were HF/HNO/HO, KF(CN)$NOH/HO (Murakami's Etch), and A large number of other etchants were previously Studied. The acidic etchant produced an acicular or "needles" pattern in the (a) planes which is an etchant effect on the "lines" pattern.

Jan 1, 1965

W. H. BASSETT, * Waterbury, Conn.-Manganese should not be expected to remedy all the defects that are due to poor melting practice. It is undoubtedly valuable in helping to eliminate porosity in many of the alloys. In the copper-nickel alloys, its use is becoming almost universal, for, beside helping to make sound castings, it tends to hold the carbon in solution in the solidified alloy. GWILLIAM H. CLAMER,? Philadelphia, Pa.-I have found that manganese copper is satisfactory for eliminating sulfur and that it works very well in the crucible and when you have reducing conditions; but in a large reverberatory charge, where the conditions are oxidizing, we were not able to eliminate the sulfur.

Jan 1, 1919

The volumes of Transactions, which are published annually, contain the list of officers, rules, etc , the Proceedings, and the papers revised for final publication (In this revision, after the prelimi¬nary publication, authors are permitted to use the largest liberty , and the changes and additions made in papers are sometimes important It should be borne in mind by those who study or quote a paper in the preliminary edition, that they may not have in that form the ultimate and deliberate expression of the author's views It should be added, however, that in the majority of cases there are no important changes) These volumes are for sale as follows, in paper covers

Jan 1, 1910

By F. N. Rhines, W. S. Pellini

In many of the otherwise well established alloy phase diagrams the solidus curves (temperatures at which liquid first appears upon melting) have not been located accurately, chiefly because the experimental techniques that have been most popular for determining solidus temperatures have been both cumbersome and subject to large errors. C. E. Homer and H. Plummerl have described a sensitive and at the same time a very simple technique for locating the solidus curves in a number of alloys of tin. Their method consists simply in noting the temperature at which a specimen of the alloy ruptures under the influence of a light bending force. Although this method is not new, it has been little used for this purpose in the past; nevertheless, it appears so attractive in its possibilities of speed, simplicity, and precision that the investigations presently to be described were undertaken to verify its merits. The redetermination of the solidus and eutectic temperatures of the lead-antimony system was employed as a medium of experimentation. New values obtained in this way are believcd to be sufficiently precise to warrant a revision of the currently accepted lead-antimony phase diagram (Fig. I). Determinations of the solidus of the lead-rich lead-antimony alloy series have been published by X. S. Dean2 and by E. E. Schumacher and F. C. Nix. Their points are represented in Fig. I. In their work the solidus was not located at antimony collcentrations greater than 2 per cent; the curve was presumed to meet the eutectic horizontal at an antimony concentration of about 2.5 per cent. In the present studies the solidus has been traced to 3.5 per cent, where the eutectic horizontal is intersected (Table I and Fig. I). Within the range investigated by Dean and by Schumacher and Nix the agreement with their values is good. H. Seltz and B. De Witt,4 on the basis of activity measurements, have calculated that the intersection of the solidus and the eutectic reaction horizontal should lie at 3.86 per cent of antimony. The following determinations of the eutectic temperature have been reported: Roland-Gosselin,5 228°C.; Ewen,6 228OC.; J. E. Stead,7 24g°C.; Campbell,8 228°C.; W. Gontermann,9 245' to 252°C.; R. Loebe,lo 245°C.; E. Heyn and 0. Bauer,ll 245°C.; H. Endo,12 250°C.; R. S. Dean,= 247' to 258°C.; E. Abel, O. Redlich, and J. Adier,13 245°C.; W. Broniewski and L. Sliwowski,14 250' to 252°C.; H. Seltz and B. De Witt,4 25o°C. A temperature of 247°C. appears to have been generally accepted in recent years; it is the value most frequently obtained by the method of cooling curves. Values below 247°C. have usually been obtained by inferior cooling-curve techniques; those above 250°C., by the method of heating

Jan 1, 1943

By W. S. Pellini, F. N. Rhines

In many of the otherwise well established alloy phase diagrams the solidus curves (temperatures at which liquid first appears upon melting) have not been located accurately, chiefly because the experimental techniques that have been most popular for determining solidus temperatures have been both cumbersome and subject to large errors. C. E. Homer and H. Plummerl have described a sensitive and at the same time a very simple technique for locating the solidus curves in a number of alloys of tin. Their method consists simply in noting the temperature at which a specimen of the alloy ruptures under the influence of a light bending force. Although this method is not new, it has been little used for this purpose in the past; nevertheless, it appears so attractive in its possibilities of speed, simplicity, and precision that the investigations presently to be described were undertaken to verify its merits. The redetermination of the solidus and eutectic temperatures of the lead-antimony system was employed as a medium of experimentation. New values obtained in this way are believcd to be sufficiently precise to warrant a revision of the currently accepted lead-antimony phase diagram (Fig. I). Determinations of the solidus of the lead-rich lead-antimony alloy series have been published by X. S. Dean2 and by E. E. Schumacher and F. C. Nix. Their points are represented in Fig. I. In their work the solidus was not located at antimony collcentrations greater than 2 per cent; the curve was presumed to meet the eutectic horizontal at an antimony concentration of about 2.5 per cent. In the present studies the solidus has been traced to 3.5 per cent, where the eutectic horizontal is intersected (Table I and Fig. I). Within the range investigated by Dean and by Schumacher and Nix the agreement with their values is good. H. Seltz and B. De Witt,4 on the basis of activity measurements, have calculated that the intersection of the solidus and the eutectic reaction horizontal should lie at 3.86 per cent of antimony. The following determinations of the eutectic temperature have been reported: Roland-Gosselin,5 228°C.; Ewen,6 228OC.; J. E. Stead,7 24g°C.; Campbell,8 228°C.; W. Gontermann,9 245' to 252°C.; R. Loebe,lo 245°C.; E. Heyn and 0. Bauer,ll 245°C.; H. Endo,12 250°C.; R. S. Dean,= 247' to 258°C.; E. Abel, O. Redlich, and J. Adier,13 245°C.; W. Broniewski and L. Sliwowski,14 250' to 252°C.; H. Seltz and B. De Witt,4 25o°C. A temperature of 247°C. appears to have been generally accepted in recent years; it is the value most frequently obtained by the method of cooling curves. Values below 247°C. have usually been obtained by inferior cooling-curve techniques; those above 250°C., by the method of heating

Jan 1, 1943

By P. Pollard

A method has been developed for evaluating acid treatments in fractured limestone fields by breaking down pressure drawdown into three component parts: (I) pressure differcntial across "skin" near the borehole face, (2) pressure differential due to flow resistance in the coarse communicating fissures and (3) pressure differential between the fine voids and the coarse fissures. It is apparent that in most successful acid treatments the first term, skin resistance, has been reduced or eliminated. Further, it is often possible to estimate the volume of coarse fissures associated with the second term, coarse fissure flow resistance. In cases where this volume is comparable with practical acid volumes it seems likely that this resistance also may be attacked with a suitably retarded acid. INTROD UCTION Acid treatment has been successfully applied as a general practice in the limestone wells in the Mara/ Maracaibo districts of Venezuela for some 10 years. At the same time the need has been felt for a more precise method of: (1) evaluating the effect of an acid job and (2) selecting wells which should benefit from an acid treatment. The following method, based on an analysis of build-up curves for wells producing from fractured limestone, provides a means of forecasting the effect acid will have on a well and in many cases the probable order of production rate increase which may be expected. In certain cases it is also possible to calculate the fissure volume through which the acid has to be displaced for best results. Various approximations are introduced in the method, but within the limitations of these the analysis gives an indication of how a well, whether previously acidized or not, may be expected to respond to acid treatment. Suitable build-up curves cannot be obtained on "tight" wells which do not give sustained production and the method is not applicable to such wells. Figs. 1 through 7 illustrate various types of build-up curves obtained from limestone wells in Western Venezuela. Curves are included showing (1) both skin and coarse fissure resistance, (2) skin resistance only, (3 and 4) reduction of skin resistance by acidization, (5) fissure resistance only, (6) reduction of coarse fissure resistance by acidization, and (7) acidization failure. This theory has been successfully applied for over three years during which 22 acid treatments have been carried out specifically to reduce skin resistance and three treatments to reduce coarse fissure resistance. The method has been found to be a useful aid in the selection of wells for acidization.

By L. W. Strock

Metallurgists handling lead and zinc ores have long been familiar with the spectrograph as a routine analytical tool, as its earliest regular use by American industry was in controlling impurities of zinc metal and its alloys. This application has been extended to other metal industries on an extensive scale, accompanied by refinements of procedure to such an extent that a large part of some metals produced, especially magnesium, aluminum and steel, are checked only by spectrographic methods for conformity to specifications. The spectrographic analysis of ores and other poorly conducting powdered solids presents difficulties not encountered with metallic samples, which can be arced or sparked as self-electrodes or can be readily dissolved, so that their solutions can be analyzed, as in the American Society for Testing Materials standard methods for zinc and zinc-base alloys. Spectra of powdered solid samples can be prepared by using carbon electrodes provided with a crater of suitable size, into which the sample is packed. Ore samples and many other powdered solid materials usually analyzed in the chemical and metallurgical laboratory are more complex and varied in composition than samples of metals produced in large tonnages. 'lore preliminary work therefore is usually necessary in devising a spectrographic method for analyzing a given type of powdered sample than for analyzing metal samples, in order to use that method with confidence. The howledge that the standard samples and unknowns produce equivalent line intensities at equal concentration is the fundamental basis of any quantitative spectrographic method. On the other hand, powdered samples have an advantage over metals in that any desired number of chemical compounds can be mixed dry in any desired ratio to produce a synthetic standard. Expcrience has shown, however, that spectra of elements in finely divided compounds introduced into a standard in preparing a synthetic ore sample do not always behave in the electric arc in a manner that produces spectral line intensities similar to those observed at the same concentration in a natural mineral. In ore samples minor elements frequently are contained in the crystal lattice of larger particles of an abundant ore mineral. Their dissociation and volatilization from the sample into the arc then proceeds differently in the standard and sample, with resultant differences in intensity. During the past 10 years I have devised and applied several quantitative spectrographic methods for determining various elements in rocks and minerals in connection with studies on their geochemistry,' but the incentive has gradually changed since the summer 0. 1940 to the specific practical problem of searching for domestic sources of rare and stratcgic metals. The

Jan 1, 1949

By W. Chubb

By measuring the hardness of metals at temperatures just above and just below their allotropic change point, it has been established that crystal structure has a real effect upon the strength of metals. The DPH of cobalt, iron, titanium, uranium, and zirconium have been measured at temperatures up to 1000°C. It was found that the body-centered-cubic crystal structure is always the softer structure when it is involved in an allotropic transformation. The close-packed and more complex structures are inherently harder, and may be expected, therefore, to be better base materials for high strength alloys. IT has been observed that for metals with nearly the same melting point (i.e., tin and lead, magnesium and aluminum) the metal with the more complex crystal structure has a higher tensile strength and hardness. It might be asked whether this effect is really caused by the difference in crystal structure; and, if so, just what is the contribution of crystal structure to the strength of these metals. A qualitative answer to these questions can be obtained by measuring the change in hardness produced by the change in structure in metals exhibiting allotropic forms. The evidence for changes in mechanical properties during allotropic transformations is rather meager. In 1909, Rosenhain and Humfrey' observed that "ß" iron showed much less deformation at the transformation temperature than a iron. By means of a torsion test, Lee found that iron bars were "critically plastic" at the a-7 transformation temperature. Sauerwald and Knehans have shown that the dynamic hardness of iron increases between 900" and 1000°C. In 1930, Albert Sauveur' presented data on the hardness, tensile strength, and torsional strength of pui-e iron up to 1000°C. He concluded, "At 900°C, the a iron transforms into y iron, and this is accompanied by increased strength and stiffness and decreased ductility." The same year, Schischokin" obtained data on the hardness of thallium at temperatures above and below its transformation temperature. His data are replotted on semilogarithmic coordinates as Fig. 1. The fact that his data fall on straight lines in this type of plot is believed to attest to the purity of his metal and the accuracy of his results. In 1941, Nadai and Manjoine" obtained tensile data on pure iron with an indicated increase in strength at about 900°C. These experiments make it quite evident that changes in mechanical properties occur when a metal transforms from one crystal structure to another; but, except for Schischokin's data on thallium, none of the measurements seem accurate enough to determine the relative magnitude of the mechanical property change. Materials The metals that have been examined for changes in hardness during transformation include l—as- deposited commercial electrolytic cobalt about 99.7 pct pure, 2—Armco ingot iron, 3—are-melted iodide titanium of a purity in excess of 99.8 pct, 4—uranium of a purity in excess of 99.5 pct, 5—are-melted iodide zirconium of a purity in excess of 99.8 pct, 6—annealed, 0.08 pct C, rimmed steel, and 7—commercially pure RC55 titanium. While the purity of the first five of these materials leaves something to be desired, it will be noted that the observed hardness discontinuities occurred at the accepted transformation temperatures. (These temperatures are indicated by vertical arrows in Figs. 1 and 3 through 7.) The last two materials are commercial alloys introduced to show the effect of minor alloying elements upon the hot hardness curve. Apparatus Hardnesses at elevated temperatures were determined by means of a vacuum hot hardness machine. A diagram showing the basic features of this machine appears as Fig. 2. This machine is essentially a deadweight hardness .machine in a furnace within a vacuum chamber. The sapphire-tipped indentor

Jan 1, 1956

By W. H. Adams

During the years when Americans were most active in investigations of the many substances containing nitrogen or ammonia, viz.: 1869 to 1875, my connection with certain chemical industries led me to experiments in the direction of the recovery of wastes from coal-gases. I take from my notes such memoranda as I think will be of interest, in the hope that some benefit may be derived therefrom by engineers at present attempting to utilize the waste products from coke-oven and blast-furnace gases. An examination of the conditions governing the manufacture of gas along the Atlantic seaboard, and an intimate knowledge of the mine-products used by the different large works, naturally led me at first to consider the well-known foreign methods of concentrating the available soluble salts in a modicum of water. The result was sufficiently promising to warrant a full line of experiments. At that time, no attention seemed to have been paid to the values of " gas-liquors." Nearly every gas-works in the United States wasted its wash-water in the sewers. The nitrogen in bituminous coals varies in quantity from 0.75 to 1.50 per cent. of the total weight. In the process of distillation in

Jan 1, 1887