Search Documents

By R. E. Ogilvie, H. C. Gatos, R. E. Hanneman

The effect of high pressure on the stability of the (any phase transformation in the Fe-V system was studied by experimental and theoretical methods. The maximum solubility limit of the y loop of the atmospheric phase diagram was found to increase by a factor of five at 40 kbars pres-sure. The solubility limits of (Y and y phases are calculated on an approximate thermodynamic basis at pressures of 20, 40, and 50 kbars as a function THE high-pressure behavior of the a =^ y transformation in iron and iron-base alloys has been the subject of considerable interest recently. For those binary or higher-order alloy systems possessing a closed y loop, the effect of pressure is to extend the region of solubility of the more dense y phase. Although quite accurate calculations have been made of the a y temperature-pressure diagram of pure iron,' only very approximate thermodynamic calculations or experimental measurements have been made of the pressure dependence of a ^ y equilibria in binary systems exhibiting a y loop.2"4 of temperature and are found in excellent agreement with experimental results. The experimental high-pressure phase diagrams were determined using binary diffusion couples diffused under simultaneous conditions of high pressure and temperature and analyzed with an electron microbeam probe. Approximate calculations of the stabilizing effect of high pressure on the o phase are qualitatively confirmed by experimental results. These previous calculations have primarily dealt with the slopes of the allotropic a (Y= y phase boundary at terminal solubility. The lack of detailed understanding or accurate experimental results of the pressure dependence of the two-phase a ^ y field has been due, in part, to the types of experimental methods previously employed. The primary purposes of the current paper are twofold: 1) to develop and make use of thermodynamic expressions with the aid of supplementary data, to approximately calculate the pressure dependence of the entire y loop and the two-phase ((Y + y) width in the Fe-V system; and 2) to accurately determine the corresponding experimental high-pressure phase diagrams. The current paper describes the powerful method used which enables the simultaneously measurement of phase equilibria and diffusion under high pressure and temperature. A second paper, part 11, will deal with the effect of high pressure on binary diffusion in the Fe-V system.

Jan 1, 1965

By G. H. Ruggles

POPULAR opinion, as it might be termed, has always been of the trend that a flotation reagent added to the ball mill during grinding would be more thoroughly mixed with the pulp and for that reason more effective in the production of low tailing. That there are other effects, inimical to good flotation, when using so-called chemical reagents, is brought out by the series of tests outlined in Table 2. It was defi-nitely proved that if either the T. T. mixture (20 per cent thiocarbanalid-80 per cent orthotoluidin) or po-tassium xanthate were added to the ball mill the result-ing flotation concentrate would be lower in copper and higher in insoluble than the concentrate produced by adding these same reagents without the ball mill cir-cuit. With the T. T. mixture four sets of tests were made. The screen analyses of the flotation feed show that there was very little difference in the original grind-ing. When the T. T. mixture was added to the head of the flotation machine the flotation concentrate had a little over 61 per cent solids -200 mesh. If the mix-ture was put into the ball mill the flotation concentrate had but 40.7 per cent of the solids -200 mesh for one set of tests, and 49.0 per cent for the other set. With the mixture at the head of flotation the total concen-trate was high in copper (34.715 and 36.525 per cent) and low in insoluble (13.20 and 11.61 per cent). The assay of the concentrate when the T. T. mixture was introduced into the ball mill was what might be termed low in copper (29.389 and 30.833 per cent). In one of these 'sets of tests (periods 8 to 11, third column) the insoluble was high, 16.81 per cent. The other run (peri-ods 12 to 15, fourth column) for some unknown reason shows a low insoluble, 12.72 per cent. With similar grinding the addition of potassium xan-thate to flotation produced a concentrate having 62.8 per cent -200 mesh, whereas with the potassium xanthate added to the ball mill the flotation concentrate was very coarse, only 36.4 per cent passing 200 mesh. The difference in the total assay of the concentrate is remarkable ; 35.847 per cent copper when the xanthate went to flotation and 30.44 per cent copper when the xanthate was added to the ball mill; insoluble, 10.94 per cent in the former instance, as 22.15 per cent in the latter.

Jan 8, 1927

By O. J. C. Runnalls, L. M. Pidgeon

J. M. Blocher, Jr. and I. E. Campbell (Battelle Memorial Institute, Columbus, Ohio)—Since the de Boer-Van Arkel process for making titanium metal involves a number of steps in a fairly compact unit, it is difficult to determine simply which of the steps is rate controlling. In any statement as to which step constitutes the rate-controlling process, qualifications appear to be in order. It is possible to design a reaction bulb in which any one of a number of steps is made to be controlling. I—With the filament removed some distance from the crude, as in the case of the authors' experiments, the interdiffusion of iodine and iodide may be controlling. 2—If, as is usually done, the crude metal is placed in a perforated cylindrical basket, or as a briquetted mass, in close proximity to the filament, the rate of deposition is increased (we obtained rates of deposition 5 to 10 times those cited in the authors' paper), and another rate-limiting factor, such as the reactivity of the crude, may take over. In this regard, we have noticed radically different rates of deposition with different crudes, and with crudes in various stages of exhaustion. 3—With a very reactive crude metal and with optimum practical geometry, still another process may be controlling. It is felt that this is a diffusion process in the immediate vicinity of the filament involving the fundamentally adverse situation of a net flow of particles away from the filament. The separate experiments on the reactivity of iodine with titanium are interesting but somewhat inconclusive. Data is still needed on the partial pressure of iodine in an operating decomposition bulb. A knowledge of the gradient of iodine partial pressure from the crude to the filament would be particularly enlightening. Optical absorption may be a useful technique here. Accurate measurements of the total pressure within a decomposition bulb under various conditions would be quite revealing. Preliminary measurements have been made at Battelle in following this line of attack. It is interesting to note that the authors' data on the temperature dependence of deposition rate indicate that the overall rate is not controlled by the kinetics of the decomposition reaction at the filament: TiI1 ? Ti + 4I Any reasonable estimate of the activation energy of this reaction would, if its kinetics were controlling, dictate a much greater temperature dependence than is observed here. The authors apparently attribute the drop in deposition rate (eventually to zero) with increased TiI4 pressure solely to a decrease in diffusion rate. However, there is an equilibrium factor involved here that must not be overlooked. As the partial pressure of TiI4 is increased, a point is reached where, due to the competing reaction of the tetraiodide with titanium to form lower iodides, the equilibrium partial pressure of titanium is reduced to the point that it equals the vapor pressure of titanium at the filament temperature and the deposition rate falls to zero. This effect would

Jan 1, 1953

By G. E. Murray

Lead blast-furnace work at Trail is unique in that this is the only plant in the world where blast-furnace smelting on a large scale for both lead and zinc recovery is carried on under one management. On this account the factors that determine economic practice differ from those of other lead smelters. In addition to this different metallurgical outlook, a great deal of structural investigation has been carried on, which has resulted in the development of a furnace which should prove of interest to all who are faced with similar problems. This description may be conveniently divided into various heads as follows: (1) General—make-up of charge, etc.; (2) structural—(a) hoods and charging methods, (b) shaft construction, (c) crucible construction; (3) handling slag; (4) handling bullion; (5) metallurgy. The Charge The Trail plant is an old one, on a congested site. As with most old plants, this limits the method of charge preparation. In general, lead metallurgists will agree that sinter when it reaches the blast furnace should contain as small an amount as possible of actual fines. There would be some difference of opinion as to the maximum size as well as of the minimum required, but to obtain the optimum condition some form of screening is indicated. This screening should take place immediately before the blast furnace if possible, and because sinter deteriorates in storage there should be as little as possible. There should also be the minimum amount of handling between the sinter machines and the furnaces. Unfortunately, at Trail the sinter must be handled considerably before it is charged to the furnace, and no feasible scheme of screening has yet been devised. Trail practice, then, demands that the sinter be a strong one physically. Dependent upon the amount of lead in it, it has been found advantageous to incorporate granulated slag into the final sinter, the amount varying inversely as the lead content. The addition of this slag makes a harder sinter, which arrives at the blast furnace in a better condition, but it entails some lack of efficiency, because desulphuriza-tion is not so rapid nor so complete.

Jan 1, 1937

By W. B. Mather

A SURVEY of the technical literature concerned with oil well drilling methods and particularly with rate of penetration by various cutting media on different types of rock provides a mass of conflicting data. This is especially true with respect to, (1) the relative efficiency of diamond, rotary and percussion drilling operations; (2) the costs of the various types of drilling; and (3) the hardness factor of various types of rock and cutting media. The latter is the particular phase of the subject discussed here. The cause of the confusion may be attributed partially to a lack of 'basic knowledge concerning the physical properties of the cutting media and of individual types of rock. It is also due in part to a general lack of uniform standards in the industry for evaluating the hardness versus drillability of rocks while possible errors in interpretation by the authors of the various papers pertaining to the subject may be an additional cause of misunderstanding. The hardness of a mineral is defined by Dana' as "the resistance which a smooth surface offers to abrasion." Webster' states that hardness is "the cohesion of the particles on the surface of a body (as a mineral) as determined by its capacity to scratch another or be itself scratched." Rock hardness, although not usually defined in publications describing rocks, is assumed to be the same as the minerals which compose the rock or the resistance of the rock to abrasion. Drillability of a rock may be defined arbitrarily as the rate at which rock is penetrated by a definite type of drilling tool with the assistance of a specific type of cutting surface or medium and under speci- fied conditions as to speed of rotation and applications of pressure. Eventually the term penetrability may have to be employed to include any method of making boreholes in rocks, since methods other than those using conventional cutting surfaces are already in operation. A case in point is the jet piercing methoda which employs an oxy-acetylene flame as a means of penetration. The word hardness as used by the drilling fraternity has a variety of meanings which depend upon the type of drilling method employed. For example, in diamond drilling, hardness is interpretated as resistance to abrasion. In percussion drilling the term implies resistance to impact or indentation, while in rotary drilling, hardness is considered anal-agous to compressive strength. The three types of hardness—abrasion, impact and compression—are conflicting variables for different types of rock. Nevertheless, the term hardness is applied indiscriminately by the industry for the resistance of rock to penetration by any type of drilling technique. Abrasion Hardness Since 1818, Moh's scale of hardness, although only relative in nature, has been accepted universally as the method of measuring mineral and therefore rock hardness. In 1933, Ridgway, Ballard and

Jan 1, 1952

By Raymond Wilson

Grinding costs are an important item in cement manufacture, and the cost of power is one of the large items in grinding costs. Even where power is of secondary importance, cost items dependent on mill capacity are influenced by the efficiency with which the mill uses power. Tube mills typify the grinding mills most generally used in cement plants, though other types are in use. Tube mills have been widely criticized as being extremely inefficient, and this feeling regarding them has led to many attempts to design more efficient grinding equipment. Other types may be an improvement over tube mills, but the improvement has certainly not been revolutionatry, at least as applied to clinker grinding. The very fact that there is doubt regarding the relative efficacy of various types of mills is an indication that an adequate basis for an analysis of performance is lacking. The development of methods of analyzing mill performance has been hampered by the lack of a suitable method for measuring the work actually done in pulverizing. There has been no acceptable standard to which mill performance might be compared. As a consequence, it was not known whether the margin of possible improvement in pulverizing operations was large or small. Even direct comparison of different types of mills was seldom possible because most plants had only one type of mill for each type of service. Comparisons between plants were difficult because of differences in the grinding characteristics of various clinkers. Some recent developments complete a chain of circumstances that place the cement industry in a particularly fortunate position for the study of its clinker-pulverizing operations. Modern investigators of grinding phenomena have generally agreed that the best measure of mill performance is the production of new surface. For most materials this measure of performance is largely theoretical and has a rather remote connection with the practical aims of the grinding operation. In clinker grinding, on the other hand, surface area is intimately connected with the properties conferred on the cement by grinding. Morcover, the determination of surface area is rapidly coming into routine use as a tost

Jan 1, 1938

By D. H. Baldwin, R. E. Reed-Hill

DURING the course of experiments involving oxygen equilibrations with a high-purity Pd-5 at. pct Rh alloy, the appearance of a subscale was noted. Most of the heat treatments in a pure oxygen atmosphere were performed at 900°C. The presence of the subscale was noted when the oxygen partial pressure was in excess of approximately 95 mm, up to 1 atm, the highest pressure used. According to available thermodynamic information' on the free energy of formation of Rh2O3 (the only reliably reported solid oxide of rhodium), this oxide should not be stable under these conditions, nor, of course, any oxide of palladium. Extraction of the subscale from the matrix was affected by treatment with aqua regia, and the resulting X-ray diffraction powder pattern is shown in Table I. This pattern is not that of Rh2O3, nor that of any known rhodium or palladium oxide. It can be indexed on a hexagonal lattice with a. = 5.22Å and co = 6.0Å. In addition to this unknown material, there was a weak Rh2O3 pattern. An X-ray fluorescence analysis of the powder gave 3214 palladium counts per sec and 5381 rhodium counts per sec, thus indicating the likelihood of a double oxide of palladium and rhodium. In view of the fact that the above result was obtained on a single sample, it is perhaps best not to insist upon the above ratio of about 0.6, but possibly to tentatively assume 0.5 or 1/1. The small amount of Rh2O3 in the X-ray pattern might have occurred on cooling, and it seems possible that the double oxide, below some temperature level, is not as stable as Rh2O3. To examine this point, some of the extracted double oxide was heated on a sheet of pure palladium in air at 900°C, and allowed to furnace-cool over a period of several hours. The X-ray diffraction pattern of the powder showed approximately the same intensity of Rh2O3 and the "hexagonal" oxide as before, but, in addition, a rather faint pattern of another crystalline species made its appearance. This finding again suggests partial transformation of the major (double) oxide to other oxides on cooling from 900°C. Application of the phase rule shows that only one equilibrium oxide (subscale) could have been present at temperature. Vacuum-fusion, oxygen analysis of the extracted subscale showed 7.7 ± 0.7 pct O. Combining this information with that of the X-ray fluorescence analysis suggests the formula PdRhO. This compound should have an oxygen content of 7.07 pct, which is within the range of error of the oxygen analysis. However, until a more careful stoichiometric study is made, it is suggested that the formula be written

Jan 1, 1965

By E. W. Parker

PROBABLY everyone is well aware that from April 1 to September 11, 1922, anthracite production was completely suspended; during those 163 days not one ton of coal was produced in the anthracite region. The production loss was about 30 million tons, and although production is now at its peak, there is no possible way by. which, within any short space of time, that deficiency can be made up. During that time the miners sacrificed in wages something over 100 million dollars. The anthracite companies paid out in cash, keeping their mines in condition to operate when mining should be resumed, something like 30 million dollars without taking in one cent of revenue. The tonnage of domestic sizes included in that lost output was about 21 million tons. The anthracite operators figured that between September 11, 1922, and March 31, 1923, they would possibly be able to produce about 60 per cent. of the tonnage that was mined the preceding year, that is, from April 1, 1921, to March 31, 1922. The problem then arose as to how that tonnage could be distributed equitably throughout the United States and Canada. We had in our records in Phila-delphia the distribution by communities, about 20,000 of them, to which anthracite had been shipped during the last five years, so that we were well posted as to what each community should be entitled to receive. We allotted to each of those 20,000 communities 60 per cent. of the tonnage that it had received during the preceding coal year, and we have endeavored to see that whatever tonnage we have been able to produce should be equitably distributed on that basis. It was a matter simply of voluntary cooperation by the anthra-cite operators who placed the distribution of their tonnage practically in the hands of the Pennsylvania Fuel Commission; the anthracite companies have almost without exception acceded to every request that we have made of them. When communities were reported entirely out of coal, a telegram or letter to the directors obligated to that community has resulted in some anthracite being shipped there, so that we have thus far kept the distribution on a fairly equitable basis. Prior to the suspension of mining operations, pre-liminary negotiations were carried on for the renewal of the wage scale, the operators thinking that it could be adjusted satisfactorily, and that the same method of procedure would be followed as during the 20 years succeeding the strike of 1902. At every termination of the wage agreement since that date, until last year, an agreement had been reached early in the season that mining operations should be continued, with the under-standing that any new agreement should be retroactive to April 1. At the meeting of the committees of anthra-cite operators and miners, on March 21, 1922, the opera-tors were presented with an ultimatum by the miners to the effect that unless an agreement were reached within ten days, mining operations would cease. That was protested against by the committee of operators as being unfair, not only to the operators and the public but to the men themselves. In spite of this protest the suspension occurred and, as you know, continued until September 11.

Jan 4, 1923

By Iley B. Browning, Louise Barton Freeman, Coleman D. Hunter

During 1942, production of oil in Kentucky reached a total of 4,169,163 bbl. of which 1,807,809 bbl. came from eastern Kentucky. This was more than a million barrels less than in 1941, owing partly to the low price of crude oil, which almost eliminated wildcatting, and partly to spacing regulations, which limited the number of wells drilled in small, shallow pools where the pressures are not sufficient to maintain maximum recovery in widely spaced wells. In eastern Kentucky much of the oil was produced from outliers of the Mauch Chunk series at the disconformable contact of the Mississippian and Pennsylvanian. Although wells producing from this horizon, known as the Maxon, are sprinkled over the entire area, the greatest concentrations are in Martin, Floyd, Knott and Pike Counties. A new 30 to 40-bbl. well has been completed in this formation in ,Pike County, where the carbon ratio is so high that ordinarily oil would not be expected. Pike County is one of the largest producers of Maxon gas, and the offset well to this oil well produced gas. Of the 412 gas wells drilled in Pike County, 12.2 per cent produced gas from the Maxon horizon. During 1942, the old Menifee " Cornif-erous" field, the Mariba-Denniston field, was redrilled between old wells, and although it did not produce any large amount of oil it did contribute 2018 bbl. In the oldest oil field in eastern Kentucky, the Ragland pool, operators are cleaning out abandoned wells and are using this oil for fuel oil. There is a possibility that some of this may be used in the future as distilled fuel oil. Eight wells were completed in 1942 in the Jackson County gas field. The development of Jackson County, which was started in 1934 and in which commercial quantities of gas were encountered at a depth of 1100 to 1200 ft., has become of importance in 1942 with the completion of eight wells, making a total of 24 commercial producing wells with an average rock pressure of 140 lb. At this time the gas is not being marketed. In the last year it has been found that these wells, which produce from the Niagaran dolomite ("Cornif-erous"), respond to acidizing and the production has been thus greatly increased. There has been less development in Estill and Lee Counties than for several years. Two wells were drilled in Greenup County, one of which had a show of oil in the Berea sandstone. One deep test, drilled by the Owens-Libbey-Owens Co. in Lawrence County, was dry. This well was drilled to a depth of 4975 ft. into the top of the Clinton shale sequence. Of the 202 wells completed in Floyd, Martin, Knott and Pike Counties, 187 were gas wells, 3 oil wells and 12 dry holes. In Floyd County 66 per cent of the gas production was from the Devonian-Mis-sissippian black shales, 53 per cent in Martin, 79 per cent in Knott and 65 per cent in Pike. This is probably the largest continuous gas field east of the Mississippi

Jan 1, 1943

By D. Weinstein, F. C. Holtz

AS a possible method of improving the elevated temperature strength properties of zirconium, an investigation was initiated on the feasibility of producing a dispersion-strengthened material. Because of the high reactivity of zirconium, its high solubility for oxygen, and the stability of the Zr-0 solid solution, the major problem in such a development is choice of a suitable dispersant. Thus, in the present investigation we were concerned primarily with the stability of various dispersants in the zirconium matrix. The experimental procedure consisted of blending powders of zirconium and a dispersant, followed by cold compaction and extrusion. The best available source of -325 mesh zirconium powder contained between 1500 and 3500 ppm Oz; to this material, powders of zirconium carbide (5 p max), vanadium carbide (5 p max), alumina (0.03 p average), lan-thana (0.8 to 2 p), ceria (0.8 to 2 p), yttria (0.8 to 2 p), calcia (44 p rnax), or thoria (0.6 to 0.8 p) were added in amounts of 7 vol pct and compacted at 65 tsi. A cylindrical compact having a density between 70 and 80 pct of theoretical and dimensions of 1 in. diam by 1-114 in. high was thus produced. After canning in copper, these billets could be extruded (5: 1) on a 54-ton capacity, slow-traverse hydraulic press with the billet temperature at 1550°F and the extrusion die at 900°F. However, lack of densifica-tion of some of the extruded billets necessitated ratios of at least 23 :1. Ultimately, all billets were successfully extruded at 1500°F to 0.190 in. diam (32 :I), fully dense rods using a 200-ton capacity press and a ram speed of 90 ipm. The microstructures of as-extruded Zr-7 vol pct LazOS and Zr-7 vol pct Y2Os are shown in Fig. l(a) and (c), respectively. These structures are similar to all the as-extruded materials and consist of an elongated, single-phase zirconium matrix dispersed with oxide or carbide particles. Very little porosity is observed, and the interface between matrix and particles appears satisfactory. The size and distribution of particles, however, are not ideally of the type desired for dispersion strengthening. Since the primary study was of particle stability with respect to zirconium, no attempt was made to overcome agglomeration during powder blending and fabrication. Some areas exhibit fine, well-distributed particles; undoubtedly, a small proportion is submicroscopic and has the

Jan 1, 1963

By A. L. Holley

THE general usage of engineers, manufacturers, and merchants, is gradually, but surely, fixing the answer to this question. In every country rails, boiler-plates, and machinery bars, whether hard or soft, are almost universally called steel, when they are made from cast ingots. Other names for the softer steels, such as " homogeneous metal," " Bessemer iron," " Martin iron," and the like, have failed to obtain general recognition. The meaning of the term steel, before it was enlarged to cover newly developing varieties, has been traced, by a recent writer, down through Percy, Shakspeare, and the Bible, in a most interesting manner, from an archaeological point of view. Undoubtedly, it did characterize hardness and other qualities imparted by carbon. It is within the memory of most of us, that all steels were tool steels, and that the soft, structural varieties were introduced-varieties which harden but little, which bend cold, and which, in many physical properties, are akin rather to wrought-iron than to tool-steel. But, since both the hard and the soft steels are made by the same processes, and have their great, distinguishing structural feature in common, viz., homogeneity resulting from fluidity, it has come to pass, despite every other proposed nomenclature, that all the compounds of iron which have been cast in malleable masses, are called steel, the term wrought-iron being still confined to malleable iron made from pasty masses, and hence laminated in structure. No inconvenience has been found, so far, in distinguishing between the more or less carburized products, in general, by the terms " high-steel," " low-steel," " tool-steel," etc., and, in particular, by prefixing the percentage of carbon and other ingredients, to the terra steel. Steels which contain distinguishing ingredients other than carbon, are called "chrome-steel," " titanium-steel," and the like, just as variously compounded bronzes are called "phosphor bronze," "alu¬minium bronze," etc. Thus the combination of several words or symbols, and figures, may completely disclose the characters of the metal, in terms that are subject to no misunderstanding. But inasmuch as several high metallurgical authorities and clever writers have of late proposed to disturb this natural and somewhat settled nomenclature, it seems important to consider the claims of the various classifications. I shall attempt, in this paper, to show

Jan 1, 1876

By William Lodding

Muscovite was the crystalline material used in the experiments discussed in this paper. It was both wet and dry ground for various periods of time. The effects (physical and chemical changes) produced in grinding are analyzed by use of thermal analysis. That grinding may change a crystalline material both in a physical and in a chemical sense has been shown by a number of authors in recent years. Mackenziel and Bartha2 reported the effects of careful grinding on muscovite, quartz, gypsum, dolomite, etc. Increase in specific surface produced by grinding implies increase in total energy of a system. Newly produced surfaces are chemically more reactive; dislocations may be introduced during grinding and, on the other hand, existing strain may be released by the same process, as shown by Holt, et a1.3 All these changes are easily detected by thermal analysis, but it is not easy to separate the multiplicity of effects registered and to arrive at quantitative interpretations. This paper is an attempt to analyze, by the use of thermal analysis, some effects produced in grinding. In differential thermal analysis (DTA) one measures the sum of all thermal changes occurring in a substance during heating or cooling; e.g., chemical changes, such as decompositions, synthesis, oxidation, reduction, etc., and physical changes such as phase transformations, changes in specific surface and thermal conductivity, strain release, etc. By thermogravimetric analysis (TGA), on the other hand, only chemical changes involving weight loss or gain are recorded. Similarly, gas evolution analysis (GEA) will register only reactions involving gas evolution. By performing two or all three of these methods of thermal analysis simultaneously and on the same specimen, one can separate the different effects registered and, by difference, evaluate their magnitude. The results of TGA are usually plotted as percent weight against furnace temp. When one differentiates weight against furnace temp, a rate of weight-change curve is obtained, and the resulting differential thermogravimetric (DTG) plots are similar in appearance to DTA thermograms for the same reaction. While the integrated area under a DTA peak represents enthalpy and can be expressed in calories per gram the area under the corresponding DTG peak represents the weight change which took place during a reaction. The similarity of DTA and DTG thermograms obtained from one material can be seen in Figs. 1 and 2. EXPERIMENTAL A Fisher mortar grinder and a porcelain mill with burundum balls were used for both dry and wet grinding. Muscovite was first carefully hand-filed and screened on 20 and 100 mesh. The middle fraction was considered essentially unaltered muscovite.

Jan 1, 1968

By M. G. Nicholas

The influence of deformation, relative movement and surface cleanliness on the strength of room -temperature "interparticle" bonds between copper surfaces has been studied. No bonding resulted when clean surfaces were merely pressed together, even under pressures of 50,000 psi. Bonding resulted, however, when clean surfaces were simultaneously pressed and moved relative to each other, some bonding occurring no matter how small the pressure or relative movement. Exposure of the clean surfaces to various chemicals inhibited bonding, none at all being produced by small relative movements. The size of the movements which first produce bonding between exposed surfaces depends on the nature of the chemical, being less than 0.002 in. for cleansing reagents and greater than 0.004 in. for lubricants, water and hydrogen sulfide. It is concluded from the experimental data that the prime requirement for bonding is the dispersal of surface films such as oxides and adsorbed contaminants. THE formation of interparticle bonds during the room-temperature compaction of powder metallurgy components greatly increases the ease of handling in subsequent production operations prior to sintering. The strength of unsintered compacts follows the same general trends as their density and hardness, but quantitative data are extremely Scarce. Quantitative correlation of the data on the overall strength of a compact with that of the individual interparticle bonds is virtually impossible due to the extremely complex geometry of powder compacts. Qualitatively, however, the strengths of unsintered compacts can be correlated with variations in parameters known to influence the extent of cold bonding, and hence interparticle bonding, such as surface cleanliness, relative movement, and deformation of the mating surfaces. Kuzmic and seelig4 found that contamination of powder particle surfaces with lubricants reduced the strength of unsintered iron and copper compacts. Interparticle shear has been shown to promote bonding by Train and Hersey7 while Gregory has shown that die rotation is beneficial. Eilender and schwalbe6 concluded that most bonding occurred during the early stages of pressing iron powder compacts when interparticle shear is one of the principal processes occurring. mile there can be little doubt that these and other factors, such as particle size and shape, affect the extent of interparticle bonding produced by compaction, evaluation of the influence of individual factors is not easy. Particle deformation and relative movement, for example, occur simultaneously during compaction, making any precise measurement of their relative influences difficult. Because of these and other difficulties encountered in studying interparticle bonding in actual powder compacts, the approach adopted in this study was to

Jan 1, 1963

By Harry W. Antes

The density changes that occurred on annealing cold-worked poly crystalline molybdenum, over the temperature range of 870" to 1630 SC, were determined. Increases in density were observed for recovery and the beginning of recrystallization. An initial decrease in density was observed during re-crystallization. A second decrease in density was observed after recrystallization was completed, as the microstructure changed from columnar grains to equiaxed gvains Both decreases in density were associated with an increase in gain boundary area to volume ratio. The second decrease in density was observed in the annealing range that immediately precedes secondary recrystallization as reported in the literature VARIOUS techniques have been used to identify the recovery, recrystallization, and grain growth processes that occur when cold-worked metals are annealed. As early as 1928 work was conducted that indicated measurable density changes occur when cold-worked single crystals of brass are annealed.' More recently, work by Murphy exhibited a corre- lation of density with microstructural changes observed on annealing cold-worked polycrystalline a brass.2 Other investigators have performed similar work on a brass and copper.324 In reviewing the literature, it was apparent that density work had been limited to fcc materials. Therefore, it was the purpose of this investigation to determine the density changes that accompany annealing the cold-worked bcc material, molybdenum. Two degrees of cold work, 30 and 90 pct reduction of cross-sectional area by rolling, were selected for this study. EXPERIMENTAL PROCEDURE High-purity vacuum arc-cast molybdenum was used in this study, the principal impurity being carbon in the amount of 80 ppm. The final rolling reductions were made at 1200°C in grooved rolls to provide 5/8-in.-diam rod. Density specimens 0.500 in. diam by 1.5 in. long were machined from the bar stock. The specimens were ground to the final dimensions to provide a smooth surface. Density measurements were made using a hydrostatic technique similar to that used by ~urphy.' This type of equipment permitted weighing in liquid immediately after the air weighing. During each weighing the temperature of the air and liquid was controlled to within 0.0l°C. This was accomplished by sealing the analytical balance in an air-tight brass chamber and surrounding it by an insulated wooden case. Preheated air was circulated in the air space between the brass chamber and wooden case by means of a blower. The temperature of the

Jan 1, 1964

By George Rice

THE A.I.M.E. Ground Movement and Subsidence Committee, pro-posed in 1920, held its first technical meeting in February 1923, under the able chairmanship of Mr. H. G. Moulton. The following list of papers and discussions, indicating the scope of the problems and relation to various conditions and method of mining, were given at that meeting by the distinguished mining engineers: J. Parke Channing, on Subsidence at Miami, Arizona; Howard N. Eavenson, on Mining an Upper Bitu-minous Seam after a Lower Seam Has Been Extracted; J. J. Rutledge, on Subsidence in Two Oklahoma Coal Mines; Benjamin F. Tillson, on Caving Cracks at the Franklin Mine, New Jersey; Dr. F. W. McNair, on the Dome Theory; William Kelly, on disadvantageous effects in Mining and Back-filling Working Upward a Steep-Pitching Iron-ore Bed; Eli T. Conner, on the good results of Back-Filling by Hydraulic Means in Preventing Destructive Subsidence in the Anthracite District; Thomas H. Claggett, on the merit of Systematic Pillar Drawing in Preventing Cracks in an Upper Seam; Henry H. Otto, successful results in the anthracite district in Mining Lower Seams before Upper Seams; Douglas Bunting, on Leading Factors Incident to Successful Mining of an Overlying Seam; Edwin Ludlow, on there being "less damage to buildings when there was complete removal of coal with complete packing than when room and pillar is used without extracting the pillars"; Edward O'Toole on "bumps" in eastern Kentucky mines, which he thought were the result of geologic stresses: H. A. Buehler, on Upheaval of Surface in an Illinois Case in Advance of the Face; and R. Dawson Hall, on The Mechanics of Subsidence from Mining. The author of this paper discussed various Winds of problems of ground movement and subsidence in both metal mining and coal mining; the production of great landslides by workings near an outcrop, as at Turtle Mountain, Alberta, Canada; and general

Jan 1, 1939

By J. M. Snook, F. C. Langenberg

FOR a better understanding of the melting and refining processes, the oxygen content of the steel bath should be determined. The oxygen content influences many process and product variables such as the efficiency of alloy recoveries, the ingot structure (through reaction with carbon in the steel), certain reaction rates, cleanliness (formation of indigenous oxide inclusions), and mechanical properties. Many methods of sampling liquid steel for oxygen have been devised. These methods can be divided into two main groups: 1) taking samples directly in the furnace or ladle;'-'0 2) removing the metal from the furnace or ladle in a sampling spoon and pouring it into a mold, or drawing the metal from the spoon into a sample holder.11-l4 The advantages and disadvantages of the two general sampling methods are presented in Table I. The bomb-sampling technique described by Huff, Bailey, and Richards8 has been used by the Crucible Steel Co. in certain research projects where oxygen contents were needed. It was recognized that a localized boiling condition could result when the mold is introduced into the steel bath, although the work of Gilbert and Bailey9 seems to indicate that the carbon boil occurring in the bomb-sampler cavity has a negligible effect on the oxygen content. In order to confirm the reported negligible effect of a carbon boil, additional work was done with adaptations of the conventional bomb sampler. The methods used are shown in Fig. 1 and are as follows: 1) Type A: aluminum wire (0.125-in. diam) coil in cavity; steel cap over mouth 2) Type B: aluminum cup in cavity; aluminum cap over mouth, 3) Type C: aluminum cup in cavity; steel cap over mouth, 4) Type D: fine aluminum wire (0.013-in. diam) in cavity; steel cap over mouth. The amount of aluminum wire in the Type A and D samples varied from 0.8 to 1.2 pct of the sample weight. The aluminum cups averaged 2.0 pct of the sample weight; the latter were used to ensure that the steel contacting the walls of the bomb cavity was fully killed. Samples were taken from plain carbon heats made in open-hearth furnaces. This grade of steel before silicon additions is essentially an Fe-C alloy and the effects of other alloying elements on the oxygen activity can be neglected. The results of sampling with the bomb samplers is shown in Fig. 2 where the percent oxygen is plotted against the percent carbon on log-log paper. Spoon sample results on the same grade of steel where the sample was killed in the spoon are shown in Fig. 3. The oxygen contents were determined by the vacuum fusion method. A comparison of Figs. 2 and 3 shows that the oxygen concentrations obtained with the spoon-sampling method (metal killed in the spoon after slag removed

Jan 1, 1960

By Sidney Powers

Since the opening of the Wheeler oil and gas field in Carter County and the discovery of oil near Lawton, Comanche County, Okla., in 1904, interest has been aroused regarding the origin of the oil in the Permian "Red Bed" region which lies between the Wichita and Arbuckle Mountains on the north and the Red River on the south. The later development of the Healdton, Loco, Duncan, Fox, and Graham fields south and west of the Arbuckle Mountains has brought the region into prominence. Recent discoveries of Ordovician and of Pennsylvanian fossils in wells in the Healdton field and of Pennsylvanian fossils in the Fox and Graham fields are of such importance from a scientific and a commercial standpoint that the occurrences and the problems arising therefrom are here briefly described. Producing oil and gas sands in the southern Oklahoma fields, with the exception of those in the Cretaceous and underlying rocks in the vicinity of Madill, Marshall County, are associated with the Permian "Red Beds" or with the underlying Paleozoic strata. In the two fields farthest south of the Arbuckle Mountains, Healdton and Loco, production has been entirely confined to sands at depths of 700 to 1400 ft. (213 to 416 m.) and only recently has a producing sand as deep as 1860 ft. (567 m.)l been encountered. These sands are found near and below the base of the red rocks and were supposed by Wegemann and Heald2 to belong in large part to the basal Permian, Wichita formation, or to the immediately underlying formations. Fossils in the blue shales and in the limestones associated with the deeper sands now prove them to be Pennsylvanian and all the producing sands at Healdton are found to be of this age. In the fields nearest the Arbuckle Mountains, the Wheeler sands at a depth of about 700 ft. (213 m.) appear to be of Permian age,

Jan 1, 1918

By J. R. Long, T. R. Graham, C. W. Matthews, R. S. Dean

In a previous paper! the authors reported on the mechanical properties of a 65 per cent copper, 10 per cent manganese, 25 per cent zinc alloy as compared with, similarly processed cartridge brass. Additional investigations by these laboratories, on higher copper alloys, have demonstrated that at lower zinc concentrations even larger amounts of pure manganese may be added to copper-zinc alloys without exceeding the single-phase solid solution limits, and that similar increases in tensile strength, yield strength, and hardness may be obtained without excessive decreases in ductility. Several compositions in this range showed also a decided color change with increasing manganese. The normal "brassy" color was considerably lightcncd and reduced to a faint yellow cast at 15 per cent manganese. With higher manganese contents the alloys were essentially white and similar in appearance to the nickel-silver alloys. From this work it appeared that it would be desirable to determine more completely the properties of the wrought and annealed white alloys. Accordingly, a more detailed study was planned of an alloy having the composition 70 per cent copper, 20 per cent manganese, and 10 per cent zinc. This alloy remained single-phase throughout the working and annealing cycles of the preliminary tests and appeared to be' about the strongest of the white single-phase alloys. The project included also an investigation of additional alloys, deviating from this composition by 5 per cent of each of the three components to evaluate the effects of variation in composition and a study of the propertics of the central alloy made with silicothermic manganese. Material Preparation Electrolytic manganese, wirebar copper, and electrolytic zinc were used for the preparation of the alloys. Representative analysis of the electrolytic manganese seldom exceeds 0.01 per cent iron, 0.02 per cent sulphur and 0.02 per cent lead, with no silicon or aluminum. A typical sample of the silicothermic manganese metal contained 2 per cent iron, 0.81 per cent silicon, 0.16 per cent carbon, and 0.36 per cent aluminum. Melting and alloying were performed in a high-frequency furnace with magnesia crucibles. Melts were deoxidized with small aluminum additions and cast into 25-lb. slab ingots. Care was exercised in deoxidation to avoid excessive amounts of residual aluminum, which has been found to have significant effects on alloys in this system. All ingots were hot-rolled at 1200' to I300°F. and then cold-rolled with intermediate anneal-

Jan 1, 1945

By Sherman L. Pease

An inexpensive and relatively rapid method that can be used by field crews is described. Fluid movement is determined by releasing a tracer (dye) in the well at a predetermined level and, after an interval of time, sampling the well fluid at another level. The testing equipment consists of a combined crusher and sampler unit that is run into the well on a wire line. The rate of movement can be calculated from time-volume relationships. Description of Method It is often desirable to determine whether there is occurring any transfer of fluid from point to point in a shut-in well, and, if so, to measure the rate of movement. When it is desired to examine a large number of wells for possible "thief" sands, the time and expense will be considerable unless the method used is inexpensive and rapid. After experimentation with several possible solutions to the problem, the Production Department of the Shell Oil Co., Inc., developed the apparatus described herein, which has proved satisfactory. Routine operations with it can be carried out by field production crews with a minimum of technical supervision and with negligible investment in equipment. The method is based upon releasing a suitable tracer in the well fluid at a known level, and recovering a sample of well fluid at another level after a measured interval of time. Repetition of this process with different time intervals between release and sampling gives the necessary data. For purposes of illustration, the setup for measuring migration of fluid in an upward direction is described in the following paragraphs. The arrangement of equipment is shown diagrammatically on Fig. I. The elements of the combination unit are the tailpiece, the crushing device, the spacer and the sampling device. The lengths of the tailpiece and spacer are varied to place the crushing and sampling devices in the desired positions in relation to the sands being tested. The crushing device breaks the glass bottle containing the tracer when the tailpiece strikes the bottom of the well and the tension on the sand line is slackened. Because of the open construction of the crushing device, the tracer is quickly and completely disseminated in the well fluid. The sampling device is a suction bailer, which obtains a sample of the fluid surrounding the perforated nipple just before the unit is picked up off bottom. The sample is retained in the barrel by the ball valve for examination at the surface. Normally, on the first run into a well, the sample is obtained near the releasing point of the tracer, and thereafter samples are taken near the base of the upper sand if migration is indicated by the dilution or absence of the tracer in the initial sample. The length of the time interval between the releasing of the tracer and the sampling of the well fluid is varied for successive runs, attempting first to establish the rate within limits and then to define it more accurately by additional runs if necessary.

Jan 1, 1946

By D. S. Sanders, E. W. Witcomb

FLOTATION tests, from which the flowsheet for the concentrator was determined, were made in a pilot mill at Chuquicamata and later comparative testing of full size flotation cells was done at the Andes Copper Mining Co. concentrator in Potrerillos. The principal sulphide copper mineral is chalcocite with varying amounts of covellite, enargite, and chalcopyrite. The oxidized portion is principally antlerite, a green basic copper sulphate. The gangue minerals include quartz, sericite, pyrite, feldspars and kaolin. Chuquicamata pit ores have proved to be hard grinding. The results of the flotation and metallurgical work prove that good extraction and concentrate grade can be obtained under a rather wide range of conditions. Metallurgy In general the metallurgy of the ore requires a fairly close control of the grind to the primary rougher flotation and of the regrind of the primary rougher concentrate before cleaning. Regrinding is necessary to reduce the insoluble content of the final concentrate since a large part of the middling combinations are between the copper and silica minerals. The alkalinity of the pulps can vary between wide limits and control of the percent solids gives the desired grind. Alkalinity Control Arroyo Salado water is supplied to the concentrator head tanks. It contains about 5000 ppm of salts but test work shows no deleterious effect. Actually this water permits a decrease of as much as 1 lb of lime per ton of ore as compared to San Pedro water, which is used for leaching oxide ore. About one quarter of the water flow through the concentrator will be new water from the reservoir. The remainder will be reclaimed from the thickeners. For primary grinding and rougher flotation, new and reclaimed water are combined in the head tanks. To avoid erratic results, only new water is used in the regrind system. Milk of lime is added to the rod mill feed chute to obtain the maximum benefit of mixing with the ore. This protects the equipment from corrosion due to entrained acids and soluble copper salts. Lime consumption is 3 to 5 lb per ton of ore. Grinding and Flotation The six bin gates over each belt feeder are opened in controlled combination and sequence to keep a live bed of ore in the bin to prevent arching and to obtain mixing. The milk of lime added ahead of the rod mill is regulated to suit rougher flotation requirements. The primary promoter reagent, Aerofloat 238, is added to the 10-mesh discharge of the rod mill as it is laundered to the ball mill scoop box. The classifier overflow is regulated to produce a grind of about 12 to 15 pct +65 mesh and 60 pct -200 mesh. A secondary promoter Z-4 (aml zanthate) and the pine oil frother are added in the overflow launder where a pH of 10 to 11 is maintained. Comparatively heavy beds of froth on the

Jan 1, 1952