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By F. J. Darnell

SINGLE crystals of a-titanium are difficult to obtain because of the phase transformation at 882 °C in which the structure changes from the high-temperature body-centered structure ß to the low-temperature hexagonal close-packed structure a. Preparation of single crystals of a-titanium has previously been accomplished by a strain-anneal method which takes several days and is not generally reproducible. Single crystals as large as 5 mm

Jan 1, 1959

In the last decade the railroads have been making tremendous strides in the development of services for the handling of bulk materials, the equipment for handling them, and the efficiency of handling, which resulted in lower costs to shippers. Pressure differential cars, giant tank cars and covered hopper cars, high capacity transloaders, and unit trains have led to substantial advances in expeditious, efficient, and economic handling of bulk materials.

Jan 1, 1973

By Eckley B. Coxe

The plummet lamp, to which I called the attention of the Institute, at the Bethlehem meeting, in August, 1871, with the improvement of the compensating ring, suggested by Mr. Heller, having come into general use for mine surveying in this country, and my attention having been called to the fact that it could not be employed in mines in which there was danger of meeting with fire-damp, I have so modified it that it can be used in all cases with safety. Mining engineers, who are in active practice in those districts where fire-damp is met with in the mines (and I am sorry to say it is becoming much more common in the anthracite regions), know how dangerous their work is when they are called upon to survey such mines, particularly when they are obliged to run lines in those parts of a mine which have been unworked, since by opening of doors, brattice, etc., to get the sights, they are liable to disarrange the currents of air, and cause any fire-damp that may have accumulated in the old workings to find its way into the levels, etc., where the party is at work. It is, therefore, very dangerous to leave an open light (such as the original form of plummet lamp) in an old breast or gangway, even when the safety lamp has shown that no fire-damp is present, for the opening of the doors, etc., may drive the fire-damp to the light, and thus endanger the lives of the engineers. The improved form of plummet lamp, now shown to you, can be used either with or without the safety apparatus. Upon the top of the plumb-bob portion of the old lamp a screw is cut, upon which a ring A is screwed. (See Plate 11.) On the external cylindrical part of this ring two small conical holes are drilled, 180' apart. The compensating ring, by which the plumb-bob part of the lamp is suspended, passes over the ring A, and is fastened to it by two small screws having conical points, which fit into the conical holes in the ring A. The safety apparatus resembles, to a certain extent, that of the Mueseler lamp. It consists of a ring B and plate C, which are united by four rods. The plate C has a cylindrical hole in the middle, and four apertures distributed radially around it. In the central cylindrical hole is fitted a conical brass chimney, which projects below the plate C, and is fastened to the latter, being kept ver-

By Eckley B. Coxe

THE plummet lamp, to which I called the attention of the Institute, at the Bethlehem meeting, in August, 1871, with the improvement of the compensating ring, suggested by Mr. Heller, having come into general use for mine surveying in this country, and my attention having been called to the fact that it could not be employed in mines in which there was danger of meeting with fire-damp, I have so modified it that it can be used in all cases with safety. Mining engineers, who are in active practice in those districts where fire-damp is met with in the mines (and I am sorry to say it is becoming much more common in the anthracite regions), know how dangerous their work is when they are called upon to survey such mines, particularly when they are obliged to run lines in those parts of a mine which have been unworked, since by opening of doors, brattice, etc., to get the sights, they are liable to disarrange the currents of air, and cause any fire-damp that may have accumulated in the old workings to find its way into the levels, etc., where the party is at work. It is, therefore, very dangerous to leave an open light (such as the original form of plummet lamp) in an old breast or gangway, even when the safety lamp has shown that no fire-damp is present, for the opening of the doors, etc., may drive the fire-damp to the light, and thus endanger the lives of the engineers. The improved form of plummet lamp, now shown to you, can be used either with or without the safety apparatus. Upon the top of the plumb-bob portion of the old lamp a screw is cut, upon which a ring A is screwed. (See Plate II.) On the external cylindrical part of this ring two small conical holes are drilled, 180° apart. The compensating ring, by which the plumb-bob part of the lamp is suspended, passes over the ring A, and is fastened to it by two small screws having conical points, which fit into the conical holes in the ring A. The safety apparatus resembles, to a certain extent, that of the Mueseler lamp. It consists of a ring B and plate C, which are united by four rods. The plate C has a cylindrical hole in the middle, and four apertures distributed radially around it. In the central cylindrical hole is fitted a conical brass chimney, which projects below the plate C, and is fastened to the latter, being kept ver-

Jan 1, 1875

By Sidney G. Parker, Jack E. Pinnell

Cubic ZnSe crystals have been grown with HCl, HBr, and I, as chemical transport reagents. The growth of large, well faceted crystals is in the order HCl < HBr < I, with some produced by I, transport being 1 cm on an edge. ZnSe:I crystals showed no strain in cross polarized light and were homogeneous as determined by electron microprobe. These ZnSe:I crystals had a mobility at 25°C of about 300 sq cm per v-sec and contained 103 dislocations per sq cm; further, these crystals were pure cubic and showed both photolumi-nescence and photo conductance. Doping was attempted during crystal growth. ZnS and Zn (S,Se) crystals were also grown by I, transport. ZnSe crystals have been grown by most of the common techniques.1"6 Of these, chemical vapor transport as developed by Kaldis2 showed promise of producing high perfection, cubic ZnSe. With chemical transport, crystals can be grown far below the transition temperature for conversion of cubic to hexagonal structure. A small temperature gradient between source and growth region tends to allow near equilibrium growth, which should lead to good crystalline perfection. Because it is necessary to form volatile compounds, halogens or their compounds are extensively used as transport agents. HCl, HBr, and I, were compared as transport agents for growth of ZnSe crystals. Doping during crystal growth was attempted. ZnS and ZnSxSe1-x crystals were also grown by chemical transport. Electrical and optical properties of the crystals were examined. EXPERIMENTAL Fig. 1 is a sketch of the growth apparatus, which was a modification of Kaldis&apos;. A quartz rod which butted against the seed crystal served as a heat sink to promote growth only on the seed. Initially, crystal growth was attempted with ZnSe prepared by wet chemical methods. Because such a material contained oxides and selenates, HC1 reacted with these oxygen compounds to form H2O and no ZnSe transport occurred. Further, this ZnSe contained about 10 ppm Cu plus other impurities. High purity ZnSe, containing small amounts or no oxygen compounds, was prepared by reaction of H2Se with zinc vapors at 600° to 800°C in an atmosphere of palladium diffused H2.7 The ZnSe thus produced was usually copper free and contained only 1 ppm by weight of magnesium as determined by emission spectrographic analysis. G.E.&apos;s electronic grade ZnS, which had about 10 ppm metallic impurities, was used without further treatment. ZnS-ZnSe charges were prepared by mixing the two compounds together, then sintering 24 hr at 1100°C in an H2S ambient. The gases, HBr and HC1, were commercial grade, of 99.9 pct purity, while the I2 was 99.999 pct pure. The single crystal seeds with (111) faces for growth were mechanically held in place by sealing the outer quartz tube to the growth tube. After the charge was introduced, the system was outgassed at l0-5 torr while heated to 500°C. The desired quantities of transport reagents were then sealed off in the system, which had been cooled to 25°C. The growth tubes were inserted into a furnace with the desired temperature and thermal gradient. The system was allowed to cool for 1 to 12 hr from growth temperatures of about 850" to 25°C. The tubes remained stationary during crystal growth. HCl CHEMICAL TRANSPORT GROWTH Preliminary runs with HC1 had a temperature gradient of 100° to 200°C and no seed or heat sink. Only small crystals were obtained in these experiments as

Jan 1, 1970

By H. R. Stahl

The ore of the Southeast Missouri lead district consists essentially of galena in dolomitic limestone. The galena usually is in a very finely disseminated condition. The experience of recent years in the concentrating plants of the St. Joseph Lead Co. has shown that dry crushing carried to a point where about 90 per cent of the ore passes a 14-mesh screen liberates the larger portion of the galena, and minimizes further necessary reduction in rod or ball mills. Concentration practice has attempted to carry size reduction to a point where economic unlocking of the galena is obtained, without causing undue sliming of the very friable galena. While 60 per cent of the tonnage of the district is treated by the flotation process, only 40 per cent of the total concentrates is produced by that means, as efforts have always been made to keep the grade and tonnage of flotation feed as low as possible. The milling practice of the district for some years has recognized the generally accepted idea of better selective grinding in rod mills as compared with ball mills, with the attendant decrease in production of fines. The function of rod and ball mills in the various concentrating plants is the grinding of table middlings and coarse tailings that carry lead values too high to be discarded. The simplified flowsheet in Fig. I illustrates the place of grinding mills in the circuit. The arrangement of classi- fiers, tables and mills constitutes a closed circuit within somewhat flexible limits. In 1937 experiments were conducted in replacing the ball charge in a 6 by 4-ft. ball mill with rods 2 in. in diameter and 51 in. long. This step was taken with some hesitancy, as it was easy to picture a mass of tangled and crossed rods. However, no difficulties developed, and after a short trial period, six more ball mills were converted to rod mills. These mills are of the spur gear and pinion, belt-driven type, using in most cases a 75-hp. motor and having a 9½-in. open trunnion discharge. As ball mills, they carried a charge of 16,000 to 20,000 lb. of balls, 2 in. in original size. The feed to the mills was dewatered by dewatering wheels and introduced at 70 to 75 per cent solids, with a single scoop feeder. One change in mill design was found advisable when rods were introduced. The existing end liners had an outward flare of 3½ in. in 12 in. These were replaced by linings having vertical interior faces, in order to prevent undue end travel of the rods. This change gave an effective working length of 52¾ in. inside the mill. No alterations were made in the shell liners, which are of the smooth type, made of manganese steel 2 in. in original thickness. The rods at present in use are 51 in. long and 1¾ in. in diameter. The composition has been varied at times; at present they contain 0.70 per cent carbon and 0.70 per cent manganese. Some breakage and etching occurs as the rods become small, but this is considered preferable to using softer rods, which may kink and cause tangling of the charge. The mill charges

Jan 1, 1947

By H. R. Stahl

The ore of the Southeast Missouri lead district consists essentially of galena in dolomitic limestone. The galena usually is in a very finely disseminated condition. The experience of recent years in the concentrating plants of the St. Joseph Lead Co. has shown that dry crushing carried to a point where about 90 per cent of the ore passes a 14-mesh screen liberates the larger portion of the galena, and minimizes further necessary reduction in rod or ball mills. Concentration practice has attempted to carry size reduction to a point where economic unlocking of the galena is obtained, without causing undue sliming of the very friable galena. While 60 per cent of the tonnage of the district is treated by the flotation process, only 40 per cent of the total concentrates is produced by that means, as efforts have always been made to keep the grade and tonnage of flotation feed as low as possible. The milling practice of the district for some years has recognized the generally accepted idea of better selective grinding in rod mills as compared with ball mills, with the attendant decrease in production of fines. The function of rod and ball mills in the various concentrating plants is the grinding of table middlings and coarse tailings that carry lead values too high to be discarded. The simplified flowsheet in Fig. I illustrates the place of grinding mills in the circuit. The arrangement of classi- fiers, tables and mills constitutes a closed circuit within somewhat flexible limits. In 1937 experiments were conducted in replacing the ball charge in a 6 by 4-ft. ball mill with rods 2 in. in diameter and 51 in. long. This step was taken with some hesitancy, as it was easy to picture a mass of tangled and crossed rods. However, no difficulties developed, and after a short trial period, six more ball mills were converted to rod mills. These mills are of the spur gear and pinion, belt-driven type, using in most cases a 75-hp. motor and having a 9½-in. open trunnion discharge. As ball mills, they carried a charge of 16,000 to 20,000 lb. of balls, 2 in. in original size. The feed to the mills was dewatered by dewatering wheels and introduced at 70 to 75 per cent solids, with a single scoop feeder. One change in mill design was found advisable when rods were introduced. The existing end liners had an outward flare of 3½ in. in 12 in. These were replaced by linings having vertical interior faces, in order to prevent undue end travel of the rods. This change gave an effective working length of 52¾ in. inside the mill. No alterations were made in the shell liners, which are of the smooth type, made of manganese steel 2 in. in original thickness. The rods at present in use are 51 in. long and 1¾ in. in diameter. The composition has been varied at times; at present they contain 0.70 per cent carbon and 0.70 per cent manganese. Some breakage and etching occurs as the rods become small, but this is considered preferable to using softer rods, which may kink and cause tangling of the charge. The mill charges

Jan 1, 1947

By Fred H. Poettmann, A. L. Benham

correlation of waters and identification of mixtures of two and three waters is important in secondary recovery evaluation studies and studies involving underground movement of waters. The importance of such studies suggests the need for a method to correlate a great number of water analyses to accurately identify and improve the understanding of mixtures of waters. Geochemical analyses of waters furnish a quantitative measure of each of the ions present in a water. Table L shows a portion of the data on many oilfield water analysis report forms in use today. Under "parts per million" are listed the quantitative amounts of each ion in milligrams per liter. Following the work of Stabler&apos; and Palmer", some laboratories have reported additional data to indicate the reaction capacity, or reacting value of each ion. Table I lists data under two subheads for the "reacting value". Under the first subhead, the reacting value is reported in gram equivalents per million, hereinafter called equivalents per million. This value is determined by multiplying milligrams per liter of the ion by a factor equal to the reciprocal of the equivalent weight of the ion. Under the second subhead (per cent) is listed the percentage of each ion based on the total equivalents per million. Sodium is not usually an analyzed value in routine analyses, but is determined by the difference between total negative equivalent per million values and the sum of all of positive ion values for which analyses were made. This difference is reported as sodium, hereafter labelled "sodium". On this basis, the subtotals of the equivalent per million and per cent reacting values of the positive and negative ions are equal. CORRELATION OF WATER ANALYSES DATA Previously reported methods for correlating oilfield waters have used part of the data in Table 1, and can be classified into two categories. Correlation by Chemical Character Correlation methods using the chemical character of waters, as represented by the per cent reacting values of the ionic constituents, have been used by Palmer2 and Tickell. These methods have the limitation of neglecting the ionic concentration of the waters. This limitation can be serious in areas where waters have the same chemical character, but differ in concentration. Correlation by Concentration of the Ionic Constituents The Reistle&apos; and the Stiff methods use the ionic concentration in parts per million and equivalents per million. These methods are effective in differentiating waters of similar chemical character and varying concentration, as in the highly saline waters of the Mid-Continent area. These methods have the disadvantage that they correlate waters by comparing many graphs of individual water analyses to determine the similarity to, or the variance from "type" waters. PROPOSED METHOD OF CORRELATING WATER ANALYSES DATA Correlation graphs presented in Fig. 1 represent water analyses data as points to facilitate the correlation of waters. The graph on the left of Fig. 1 is a plot of per cent reacting value of magnesium vs calcium. The right

By R. S. Pratt

IT is proposed to discuss the materials and furnaces, as well as the melting procedures used in preparing metal for casting billets, bars or cakes for mill fabrication. As far as possible, consideration will be given to the alloys that are commonly made in most brass mills producing strip, tube, rod and wire. RAW MATERIAL The basic raw material for such mills, of course, is copper, which may be obtained in the form of ingots, ingot bars or cathodes. Refinery-cast ingots and ingot bars, which are simply double ingots, are supplied in accordance with A.S.T.M. Specifications as regular electrolytic or fire-refined tough-pitch copper. In the wrought-metal industry, the electrolytic brands have been preferred, although during the war large quantities of fire-refined coppers sufficiently pure to be suitable for all existing requirements were imported from South America. With the exception of Lake copper, most primary fire refined coppers produced in this country have not been considered satisfactory for wrought metal alloys. Cathode copper, which is now widely used instead of ingot copper for alloying, is the electrolytically deposited metal that is normally remelted in the production of electrolytic tough-pitch ingots. It is in the form of rough, flat plates not suitable for processing but quite satisfactory for melting when sheared into suitable sizes. Raw zinc is perhaps the next most important raw material and this is obtained in various grades, depending on the analytical requirements of the alloy to be made. The grades of zinc as outlined in the A.S.T.M. Specifications vary in cost with the amount of impurities-lead, iron, cadmium-and are purchased in such a way as to produce the most economical mixture consistent with the purity required in the alloy. Other virgin metals (lead, tin, aluminum and nickel) are used in varying quantities for making copper alloys. These elements can also be purchased in accordance with the appropriate A.S.T.M. Specifications where available. Also available are a number of special alloys, which are used as deoxidizers or as means of adding relatively small quantities of elements not suitable for adding directly as virgin metal. In this category are such materials as phosphor copper or phosphor tin, silicon copper, manganese copper, cadmium copper, and copper-iron or zinc-iron alloys. Some of these alloys may be purchased on a definite alloy basis or may be produced in the plant itself for its own use. For largely economic reasons, however, a great proportion of the charge to the melting furnaces consists of alloy scrap. In the production of many finished products, as much as 70 or 75 per cent of the metal originally cast may be discarded at various points along the production line. This material eventually finds its way back to the casting shop as mill scrap, overhaul or scalping chips, skeleton scrap, rod turnings, or miscellaneous fabricating scrap. One of the most serious problems in the

Jan 1, 1946

ALTHOUGH I have already described to you the procedure for making assays of the ores (a thing that is not very different from what I wish to describe in the present chapter), I shall repeat it in substance, with the addition of the method of assaying gold, in order to tell you certain rules for weights which are very necessary to know, and above all in order to demonstrate to you the method of refining a small quantity of silver by the use of a cupel, and in order to tell you how there are (I find) only two ways that are customary for bringing silver to fineness. One is that of the cupel [copella] and the other is that of the cupeling hearth [cenneraccio], one for a small and the other for a large quantity. But although they are called by two names and appear to be two methods, the aim and the procedure of both is actually the same. Nor do I know of other difference between them than the carrying out of the method and the large or small quantity. Cupeling is a very useful thing for anyone who handles gold or silver to know. Indeed it is necessary, because it not only throws light on the work that is to be done but it also shows the truth [55] and the correct weights in large quantities. It is a quicker and easier way of bringing the work to the desired perfection than is afforded by the method for large quantities. Therefore, as you have heard, it is used in making assays in order to know exactly what quantity of the substance of silver or gold is in copper and lead or in ores, as well as in that melted material which remains among the charcoal and ashes. In short, it is the measure by which you have the certainty and safety of knowing that you have not been deceived by art or by your workmen, who had no other interest than their simple wages. Many workmen are found who are so untrustworthy that they no sooner get control of a thing than they think up some fraud, and even though some know that they must give an accounting they do not restrain themselves, although sometimes they would perhaps act with greater security and more deception than they do if they did not fear detection. For, truly, since silver is a valuable thing and every bit is worth much, a man should not enter into refining it with closed eyes. If for no other reason this pro-

Jan 1, 1942

By F. C. Oliphant, George H. Fancher

Two samples of drilling mud from the Hastings oil field, Texas, were tested, and the solids in each were separated into small fractions of a limited range in particle size. The mineral composition of each fraction by X-ray analysis is reported, and the results are interpreted in relation to other measured quantities, such as the physical properties of the original samples and the density of the various fractions. It was found that only 7 to 8 per cent by weight of the solids was of colloidal dimensions and that neither of the samples contained montmorillonite but did contain illite. Considerable calcite was also found. These data should be useful to the geologist interested in the origin and history of sedimentary strata as well as to the petroleum engineer. Introduction The questions, What is good drilling mud? What constitutes bad drilling mud? are pertinent, because the proper use and control of drilling fluids has been a factor of great importance in the successful drilling and completion of oil wells since the days of Captain Lucas. Adequate control of the characteristics of drilling fluids has assumed greater significance comparatively recently because of the problems introduced by caving formations in deep wells, costly blowouts and impressive mud bills. Much is known about the solution of some of the problems but, despite extensive research directed toward a better understanding of the physical and chemical properties of clay suspensions, it is difficult to define precisely a drilling mud, and much more difficult to say what constitutes a good mud. It is generally believed that the smaller particles of a drilling mud greatly affect its physical properties. In fact, it is customary to blame the colloids in a mud for nearly everything that goes amiss, because colloidal properties have effects out of all usual proportion on viscosity, filtration rate and reaction to electrolytes. It is germane to know whether drilling muds possess colloids and if so, the quantity and kind. Source oF Samples Two drilling muds from the Hastings oil field, Brazoria County, Texas, were selected because it is generally agreed that in this oil field good natural muds made solely from formations penetrated by the drill can be used until the well is nearly ready for completion. Customary drilling procedure in this field is to spud in with water, set a protective string of pipe, drill to 2500 ft. and set the surface casing. Drilling is continued to 5500 ft. with no treatment of the drilling fluid other than addition of water to

Jan 1, 1943

By F. C. Oliphant, George H. Fancher

Two samples of drilling mud from the Hastings oil field, Texas, were tested, and the solids in each were separated into small fractions of a limited range in particle size. The mineral composition of each fraction by X-ray analysis is reported, and the results are interpreted in relation to other measured quantities, such as the physical properties of the original samples and the density of the various fractions. It was found that only 7 to 8 per cent by weight of the solids was of colloidal dimensions and that neither of the samples contained montmorillonite but did contain illite. Considerable calcite was also found. These data should be useful to the geologist interested in the origin and history of sedimentary strata as well as to the petroleum engineer. Introduction The questions, What is good drilling mud? What constitutes bad drilling mud? are pertinent, because the proper use and control of drilling fluids has been a factor of great importance in the successful drilling and completion of oil wells since the days of Captain Lucas. Adequate control of the characteristics of drilling fluids has assumed greater significance comparatively recently because of the problems introduced by caving formations in deep wells, costly blowouts and impressive mud bills. Much is known about the solution of some of the problems but, despite extensive research directed toward a better understanding of the physical and chemical properties of clay suspensions, it is difficult to define precisely a drilling mud, and much more difficult to say what constitutes a good mud. It is generally believed that the smaller particles of a drilling mud greatly affect its physical properties. In fact, it is customary to blame the colloids in a mud for nearly everything that goes amiss, because colloidal properties have effects out of all usual proportion on viscosity, filtration rate and reaction to electrolytes. It is germane to know whether drilling muds possess colloids and if so, the quantity and kind. Source oF Samples Two drilling muds from the Hastings oil field, Brazoria County, Texas, were selected because it is generally agreed that in this oil field good natural muds made solely from formations penetrated by the drill can be used until the well is nearly ready for completion. Customary drilling procedure in this field is to spud in with water, set a protective string of pipe, drill to 2500 ft. and set the surface casing. Drilling is continued to 5500 ft. with no treatment of the drilling fluid other than addition of water to

Jan 1, 1943

By Robert E. Cuthbertson

IT is the purpose of this paper to describe in detail the laboratory development and mill application of an unusual combination of flotation reagents employed in the concentrator of the Climax Molybdenum Co., on the Continental Divide, near Leadville, Lake County, Colorado. This development originated in an ore-dressing research laboratory maintained by Climax at the experimental plant of the Colorado School of Mines, which is staffed by men directly employed by the Climax Molybdenum Co. Mill-scale testing of laboratory developments was supervised by a representative from the testing laboratory, working in close cooperation with the operating staff at the mill. General milling practice at Climax is ably described in a paper by E. J. Duggan,1 mill superintendent. Other aspects of the Climax project have been described in papers by W. J. Coulter,2 by Butler, Vanderwilt and Henderson3 by Allen Kissock,4 and by Leo H. Glanville.5 Consequently, this paper will be confined to the metallurgical aspects of recent reagent developments, avoiding, as much as possible, repetition of material covered in these earlier publications. BRIEF HISTORY OF REAGENT PRACTICE AT CLIMAX Prior to the year 1937, the only reagents employed at Climax for froth production and collecting action in the flotation of molybdenite were steam-distilled or destructively distilled pine oils. The only exceptions to this practice were brief periods of mill testing, when reagents of various types were tried on an experimental basis. None of these experimental runs was sufficiently encouraging to justify its continuation as regular practice. Sodium, cyanide has been employed since the very early days of milling at Climax as an inhibiting agent for control of pyrite and chalcopyrite. Alkaline reagents such as lime or soda ash have been used in recent years to minimize the detrimental effect of iron salts on flotation of molybdenite. The presence of these harmful salts is attributed to the decomposition of fine metallics abraded from liners and balls in the first stage of regrinding rougher concentrate. Flint pebbles are used in subsequent regrinding, since alkaline reagents are not entirely adequate to offset the inhibiting effect of iron salts as the grind becomes progressively finer and the grade of concentrate progressively higher. Climax metallurgists were familiar at an early date with the use of petroleum products such as kerosene and gas oil as promoters of flotation of molybdenite. Charles C. Oliver6 discussed the use of pine oil and kerosene as early as 1920, in connection with the milling practice at Dominion Molybdenite Co., Quebec. Never theless, the early attempts to apply this knowledge in the Climax concentrator were complete failures. In the light of recent experience, it may seem strange that the early mill tests with petroleum

Jan 1, 1944

By Lewis Reeve

As. part of a program of investigation of the properties of electric arc welds carried out in the laboratories of the A. 0. Smith Corporation, considerable work has been done on the determination of the oxygen, nitrogen and hydrogen content of different types of weld metal, employing for this purpose the so-called "vacuum fusion method." It is the purpose of this paper to describe certain improvements that have been introduced in this method of determining the gas content of metals, with particular references to the steel specimens examined in this investigation. The method and apparatus used at the beginning of the investigation were essentially those of the Bureau of Standards as described by Vacher and Jordan.1 Later a number of changes were introduced which resulted in. more rapid evacuation of the graphite crucibles employed and which enabled larger volumes of gas to be dealt with than could be handled conveniently in the Bureau of Standards equipment. In addition, the analyzing of the gases evolved from a melt in the same apparatus as collected was abandoned in favor of analysis outside the equipment using standard methods of gas analysis. The time required for gas analysis in the apparatus itself, as described by the Bureau of Standards, was found to be considerable, and during this time the rest of the equip-ment was tied up, preventing its use for the analysis of further steel sam-ples. As a result of the modifications introduced, the time required for the analysis of a steel sample for gas content was reduced from about 8 hours to less than 3 hours. Subsequently, the whole procedure of melting the sample and collect-ing the gases evolved was modified so as to enable a distinction to be drawn between the easily reducible oxides such as iron oxide and the more stable oxides such as silica and alumina. At the same time evidence was obtained indicating the probable existence in the steels of other nitrides than those of iron alone and making possible their quantitative determination.

Jan 1, 1933

By C. G. Dunn, F. W. Daniels, M. J. Bolton

IN recent papers on interface energies in metals¹,² the concept of an equilibrium of forces has been used in the measurement of interfacial tensions. Mathematically the equilibrium of three forces is given by the relations: where the 2&apos;s are the interfacial tensions (interface energies per unit area of interface) of three phases or grains meeting at angles 21 22 and 23 (212 relates to the 1-2 boundary formed by grains 1 and 2;223 to the 2-3 boundary, etc.). If these relationships are valid, one can calculate relative values of the interface energies from measured boundary angles on specimens which have been brought to equilibrium. Since Eq 1 may be derived through a mathematical process of minimizing the grain boundary energy under the restriction that the ?&apos;s be independent of boundary orientation: the concepts of surface tensions and equilibrium of forces are not particularly essential. To deal with the general case involving dependence of boundary energy on boundary orientation, it becomes desirable to drop certain concepts formerly held (namely that energy per unit area is identical with force per unit length or surface tension) and to use the energy concept alone. It is appropriate, therefore, to use E in place of ? in deriving and using the more general equations that express the anisotropic nature of the grain boundary energy. Herring3# &apos; recently has derived the required general equations using the principle of minimization of energy. Specifying the boundary orientations in terms of angles (4) measured with reference to crystal axes within the grains, Herring&apos;s equations take the form E23 + E21 cos?8 + E12 cos?2 — sin ?12 + sin?2-?E12/?12 =O [2] where the partial derivatives are measured in the direction of counterclockwise rotation of the boundaries. Eq 2 implies that an infinitesimal displacement of the triple point along the 2-3 boundary produces no change in the boundary energy. Similar equations apply for infinitesimal displacements along each of the other two boundaries. From such equations Herring obtains the following general relationship (1 + E1 E2) sin?8 + (E2 — E1) cos?3 ________ E38______________ = (1+ E2 E8) sin ?1+ (E3— E2) cos ?1 __________^5____________[3] (1 + E sin ?2, + (E1 — E8,) COS ?2 1 E28 where E1 = 1/E23- E25 and PC and c8 have similar expressions. It is apparent that Eq 3 reduces to Eq 1 when the c&apos;s vanish. Eq 3 also reduces to Eq 1 when the E&apos;S are all equal. Shockley and Read&apos; have pointed out one limitation to these equations. When E plotted versus 4 appears as an energy cusp, as their theory requires, for example, for the energy near a twin boundary position, then Eq 3 (and therefore Eq 1 also) no longer applies if one boundary is in the minimum energy position. One of the equations of form Eq 2, however, applies if the infinitesimal displacement is along the boundary associated with the energy cusp. From the foregoing treatment it will be apparent that equilibrium angles alone are not sufficient in general for calculating relative interface energies.

Jan 1, 1951

By D. J. Salley, M. Burke, G. L. Simard

A PREVIOUS paper1 described experiments on the interaction of dithiophosphate with galena and suggested that the process had characteristics of both chemisorption and surface chemical reaction. In order to add to this knowledge, a study has been made of the competition of a second ion with the dithiophosphate for a galena surface. Use again was made of radiotracer methods. Since radiophosphate was readily available, it was chosen as the competing ion. It is a feature of the tracer method that, in spite of similarity in the chemical behavior of the ions, the measurement of one ion in the presence of another can be made as simply as if only one ion species were present. In order to study the competition effectively, it naturally was necessary to examine the interaction of phosphate with galena alone as well as in the presence of dithiophosphate; consequently, this report consists of two parts. The first is devoted to a study of the rates, the isotherms, the desorption, and the exchange in the phosphate-galena system in the same manner as was done for the dithio-phosphate-galena system. The second portion is concerned with the studies on the competition. Flotation experiments on the three-component sys- tem are also outlined and the relationships involved are discussed briefly. The experimental method was that of the previous paper. The preparation of the galena, the radioactive and the nonradioactive dithiophosphate, and the procedures for radioactive counting, for sorp-tion, and for flotation measurements were identical to those previously employed. The radiophosphate* was used in the form of disodium phosphate solution. In the competition experiments the effect of the phosphate ion in depressing dithiophosphate uptake was followed by holding the initial concentration of nonradioactive phosphate constant while varying the initial concentration of the radioactive dithiophosphate. Counterfashion, the depression of phosphate by dithiophosphate was obtained by keeping the initial nonradioactive dithiophosphate ion concentration constant and altering the initial concentration of the radioactive phosphate ion. All solutions were buffered at a pH of 7.8 a0.1 by 20x10-&apos; mol per cc of sodium carbonate. Measurements with radiocarbonate indicated that little or no carbonate could be sorbed in the presence of

Jan 1, 1952

A method has been developed to remove calcite from the leaching circuit in the uranium in situ leaching system. The process involves injecting the leachate and a pH control agent tangentially into an inverted cone reactor containing calcite seed catalyst. The leachate can be treated at high throughput to obtain clear effluent containing 5 ppm or lower Ca. Both lime and ammonia are effective pH control agents and consumed according to stoichiometry.

Jan 1, 1985

By R. E. Miner, J. K. Jackson, D. F. Gibbons

Internal-friction measurements were made during isothermal aging treatments of 18 pct Ni maraging-steel wires between 420° and 612°C. A sharp initial drop in the internal-friction level was interpreted in terms of a rapid dislocation recovery reaction. The rate of the recovery was found to be independent of temperature. Truncation of the recovery reaction was apparent in those systems that exhibited the rapid age-hardening characteristics of the maraging steels. It is proposed that this initial hardening response is the result of a low activation energy preprecipitation reaction involving molybdenum. A gradual rise in the internal-friction level at longer aging times was associated with the precipitation of a molybdenum-containing precipitate. CONSIDERABLE research effort has recently been devoted to the mechanisms responsible for the high strength and toughness of 18 pct Ni maraging steels. These bcc martensitic alloys are found to harden during aging at temperatures between 400° and 600°C. The aging response is very rapid with more than half the total hardness increase occurring within the first few minutes of aging, Fig. 1. Precipitate particles have been observed in the later stages of aging by a number of investigators.&apos;-&apos; While the identity of the precipitates remains the subject of some controversy, one or more of the intermetallic compounds, Ni3Mo, Ni3Ti, and Fe2Mo, are almost certainly involved. Heterogeneous nucleation of precipitates at dislocations has been noted8 and cobalt is believed to enhance the formation of fine, homogeneously distributed particles by lowering the solubility of the alloying elements in the martensitic matrix.3,7 Transmission electron microscopy studies of the initial hardening behavior have not been fruitful. Strengthening mechanisms based on atomic ordering have not been generally supported by X-ray and neutron-diffraction experiments.9 In the present investigation, the aging reaction was studied using isothermal-aging internal-friction measurements. The marked sensitivity of internal friction to short-range diffusion and precipitation processes has provided a convenient tool for the elucidation of the strengthening mechanisms operative in the maraging steels. EXPERIMENTAL PROCEDURE An upright torsion pendulum was used to measure the internal friction of several maraging steels during isothermal aging. The pendulum was placed in an atmosphere of helium at a pressure slightly less than atmospheric. To permit measurement of internal friction during the first minutes of aging, the specimens were rapidly heated by passing a current through them in a manner similar to that described by Ang and Wert.10 Thermal gradients in the specimen were largely eliminated by using specially designed specimen grips11 which produced temperature variations of less than 1 pct over 90 pct of the specimen length and less than 3 pct over the entire length at aging temperatures up to 620°C. A proportioning strip-chart program controller was employed to maintain constant specimen temperature during treatments of up to 36 hr duration. A number of vacuum-melted laboratory heats having compositions near that of a typical commercial 18Ni-7Co-5Mo-0.4Ti alloy were investigated. The amount of cobalt was varied from 0 to 7 wt pct in five of the heats. Either molybdenum or titanium was omitted in the remaining two heats. The alloy desig-

Jan 1, 1967

By Stanley Herold

AT THE present time five localities in the Argentine Republic are known to bear direct evidences of the presence, of petroleum. The segregation of these localities is more or less arbitrary inasmuch as minor indications may be found to extend from one locality to the other at no regular distance apart, especially in the northern and western part of the republic. These localities are listed as follows: North Argentine-Bolivian region, Salta-Jujuy district, provinces of Mendoza and Neuquen, Comodoro Rivadavia, and the Gallegos-Punta Arenas region. Economic conditions attract us to the possibilities of developing these and other regions of countries in the southern hemisphere. Development work will, naturally, be undertaken first in such localities as present direct manifestations of the presence of petroleum; "hidden fields" may exist, but, unless discovered by accident, their development will be left to the last. The problems to be solved in the development of the petroleum resources of the Argentine republic are mainly of stratigraphy, structure, and transportation. We are not here concerned with the unfavorable climate of the countries to the north in the tropics where, for us of the "far north," life hangs by a thread ready to be severed by a mosquito, gnat, or tropical germ.

Jan 2, 1920

By Alden B. Greninger, Alexander R. Troiano

Metallurgists have long believed that martensite in steel forms as plates along the octahedral {111} planes of austenite. Much has been written about mechanisms whereby units of the austenite lattice are pictured as transforming to martensite by shearing movements initiated along the octahedral planes of austenite, supposedly resulting in plates of martensite lying parallel to these planes of shear. A critical inspection of two or three photomicrographs of quenched hypereutectoid steel led us to the conclusion that the orientation habit of martensite, at least in hypereutectoid austenite, could not possibly be octahedral. Inasmuch as recent studies,30,31 of the martensite-type reaction in nonferrous alloy systems have established the irrational orientation habit as characteristic of this type of lattice transformation, the need for a thorough restudy of the crystallography of martensite formation in steel was evident. The present paper reports the results of such a study, extended to include both cementite and some of the products of constant-temperature decomposition of austenite. Also reported are a few of the results obtained from a microscopic and X-ray study of the austempering process in very high-carbon steel. I. The Martensite Transformation Previous Work Microstructure and Crystal Structure of Martensite.—Among the best series of published photomicrographs of quenched steels are those of Whitely,1 Robertson,2 Hanemann and Schrader,3 and Lucas.4 The crystal structure of martensite is body-centered tetragonal, with axial ratio varying from 1 near 0.0 per cent carbon to 1.08 for 1.75 per cent

Jan 1, 1940