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By E. T. Turkdogan, P. Grieveson

Experimental results are presented for the rate of solution of nitrogen in a iron in the temperature range 750° to 873°C and in 6 iron in the temperature range 1410° to 1470°C. It is shown that the rate controlling process is diffusion of nitrogen into the iron. The diffusiting of nitrogen in a and 6 iron is derived from the results, and the temperature dependence of the diffusivity is represented by the equation D = 7.8 x e- 18,900/RT sq cm per sec. The solubility of nitrogen in a and 6 iron, in equilibrium with 1 atm pressure of nitrogen, has been measured. Using these results and other available data, it is found that the variation of the logarithm of nitrogen solubility with the reciprocal of absolute temperature is nonlinear. In an Appendix, some results of Darken and Smith are presented for the rate of solution of nitrogen in iron using ammonia + hyidrogen mixtures. These data also support the view that diffudsion of nitrogen in iron is the rate-controlling process when ammonia + hydrogen mixtures are used. A considerable effort has been made to obtain data on the solubility1-5 and diffusivity of nitrogen in a iron6-l2 because an understanding of the effect of nitrogen on the properties of steel must be based on an accurate knowledge of the properties of nitrogen in pure iron. However, no information is available concerning the kinetics of solution of nitrogen in a and 6 iron. Recently the authors13 have investigated the rate-controlling mechanism operating in the kinetics of solution of nitrogen in y iron. This study was directed to determine the rate-controlling processes for similar reactions with a and 6 iron as well as to establish values for the solubility of nitrogen in equilibrium with nitrogen gas in a and a iron. EXPERIMENTAL The procedure used in experiments to determine the rate of solution in cylindrical iron rods was the same as that described in a previous communication.13 Ferrovac E grade iron used in all experiments contained the following impurities in weight percent: C, 0.005; Mn, 0.001; P, 0.002; S, 0.006; Si, 0.006; Ni, 0.025; Cr, 0.002; V, 0.004; W, 0.02; Mo, 0.01; Cu, 0.001; Co, 0.01; 0, 0.007. After cleaning the surface, the iron rods were treated in an atmosphere of purified hydrogen for 17 hr before the reacting gas was introduced for known experimental times. After quenching, the samples were sectioned radially and analyzed for nitrogen. In addition to experiments using rods, iron foils were used in the measurements of solution rates of nitrogen in a iron. The foils of two different thicknesses were prepared by cold rolling Ferrovac E grade iron cylindrical rod to 0.051 and 0.152 cm. Foil samples were used in a rectangular form 5 cm long and 1.25 cm wide. The specimens were thoroughly cleaned of surface oxide with fine emery cloth and degreased with carbon tetrachloride immediately before entry into the furnace. The experimental procedure was the same as that used in the study with rods. At the completion of an experiment, the foil samples of the nitrogenized iron were analyzed for nitrogen after discarding 0.3 cm from the perimeter of the specimen. Iron foils were nitrogenized and denitrogenized in the a and 6 range with a gas mixture of 95 pct N and 5 pct H for times varying from 5 min to 2 hr. Results obtained for the average composition of nitrogen in iron for these experiments are presented in Fig. 1. Prior to the denitrogenization experiments, the samples were saturated with nitrogen at 1000°C and 0.67 atm N, giving a uniform nitrogen concentration of 0.0204 pct. According to the known a-y phase boundary in the Fe-N system,14 this composition lies within the ferrite region at temperatures 750" to 850°C. Use of this initial nitrogen content insured that reaction occurred between the gas and a single solid phase, a iron. Examples of the results for the mean concentrations of nitrogen in cylindrical iron rods, 0.356 cm radius for both the a and 6 ranges are given in Fig. 2. Typical examples of the results obtained for the radial distributions of nitrogen in rods are presented in Fig. 3. It appears that the results for radial distributions can be extrapolated to constant surface compositions which agree with the equi-

Jan 1, 1964

By Clarence Seyler

THE technical difficulties of cutting thin sections of coal for examination by transmitted light have hitherto restricted the investigation of the important subject of the microstructure of coal to the few possessed of the requisite skill and time. Apart from this, the method fails with anthracites and other coals rich in carbon, owing to the opacity of the material. Occasional use of the method of polishing a surface, with or without etching, has been made, but it was not until Winter1 published an account of his results that attention was seriously directed to the method. In May, 1923, a specimen of dull anthracite came into my hands; I tried Winter's method on it and the presence of megaspores and other vegetable structures became clearly visible. A preliminary notice was published by me;2 but I soon abandoned the use of Schulze's solution having found that a mixture of chromic and sulfuric acids gave far better results. In the meantime Turner and Randall, in America, had independently developed the method of flame etching, as applied to anthracite, with great success. I have spent a year studying the method of chromic etching, which gives excellent results with bituminous coals and cannels, as well as with anthracite. For anthracites, I have used the chromic method and Turner's method of flame etching, whichever was the more convenient or as a check one on the other. The polishing is done, according to metallurgical practice, by the use of a polishing machine and successively finer emery paper, followed by polishing on cloth moistened with a suspension of levigated green oxide of chromium, and a final rubbing on "selvyt" (a cotton velvet polishing cloth) moistened' with alcohol. The polished sample is examined by reflected light with a 2/3 and 1/6 in. objective. Bituminous coals usually show considerable structure, and even anthracites show it faintly in places. The sample is then etched by immersion in a boiling solution made by adding 10 c.c. of concentrated sulfuric acid to 30 c.c of a saturated solution of chromic acid; enough water is then added to dissolve

Jan 3, 1925

By James K. Stanley

When a plastically deformed mctal is heated to a certain temperature, it undergoes a complete change in microstructure, the consequence of which is a marked alteration of mechanical properties such as hardness, strength and ductility. This change in microstructure occurs by re-crystallization and is a process involving the formation and growth of strain-free nuclei in the deformed matrix. These nuclei continue to form with time and grow until a new grain structure replaces the cold-worked structure. The formation of the nuclei in the deformed sheet of I per cent silicon ferrite is illustrated in Fig. I. If a recrystallization is conducted iso-thermally, a nleasurement of the fraction of the matrix recrystallized plotted against time leads to an isothermal recrystallization curve, first established in 1942.1 Such recrystallization curves are shown in Fig. 4. These curves show that the recrystallization of a cold-worked metal is best considered as a rate process rather than a time independent process such as is suggcsted by the improperly named and misleading recrystallization diagrams involving deformation, temperature, and grain size.2-5 Any study of the rate of recrystallization resolves itself into a study of the component rates of nucleation and growth. The previous paper1 provided an account of the determination of the rates of nucleation; N, the number of nuclei formed per unit time per unit of unre-crystallized area, and growth, G, the radial growth in unit time, in the recrystallization of silicon ferrite (I per cent Si). A method was developed to furnish experimental data for evaluating the effect of the recrystallization variables on N and G. The mathematical analysis for the derivation of the isothermal recrystallization curve was developed for a two-dimensional case (in thin sheets where the diameter of the recrystallized grain is greater than the sheet thickness). The present paper is a continuation of the study of recrystallization of I per cent silicon ferrite begun in 1942.1 In this work the effect of the factors deformation, temperature, grain size, composition, and recovery is studied with respect to the rates of liucleation and grouth. At the same time it is shown how the cooperation of N and G affects the isothermal recrystallization curve. The study of these variables on N and G has a definite bearing on the mechanism of recrystallization and should lay a foundation for a rational theory on the subject. Procedure The procedure used in these experiments was essentially the same as that described previously but in certain details some changes were made in the interests of speed. With few exceptions, the procedure is the same for the study of all the variables. Where the procedure is different from standard manipulations attention is called to this fact.

Jan 1, 1945

There is a Chinese saying-may you live in interesting times. Certainly we do tod.a~our mining professions. We are, of course, totally dependent on a' healthy mining industry for the chance to practice our chosen professions, and for our Institute.Let us look at one of the more interesting facts. The mining industry now accounts for some 50 per cent of Australia's exports.This massive earning of foreign exchange is the key to keeping our increasing overseas debt in check. Furthermore, mineral production..including petroleum, saves us a large amount of foreign currency by providing essential minerals, including energy minerals, for local consumption.With such fundamental inputs to our economy, any primary school student, any child in fact, should be able to see that the mining industry and mining professions are very important to our nation. Yet the average citizen is unaware of this simple fact as they enjoy their high standard'of living and think that we are still living in the lucky country.Therefore, it is most interesting to me that the average citizen, and most of our politicians, seem to hold mining and miners in low esteem. I use the term miners to describe all those important people, like us, who work in the mining professions, and are employed by, or are dependent on, the mining industry.So why are we miners in this paradoxical situation of doing wonderful works, being the backbone of the country, and yet being held in low regard by the very community we underwrite.Truly-it is interesting-or did the Chinese mean intriguing?It is indeed paradoxical that we are the rare people who open up the land, borrow small parts of it for a relatively short time to harvest the mineral crops, then return it to the community for other uses; and when we return the land back to the community at large it should be in better shape than when we started. There will be infrastructure - roads, airstrips, supplies of water and power, parks and housing-all left behind after mining.These benefits to the community are ignored while our critics focus on the small scars on the landscape which sometimes cannot be healed at reasonable cost; and yet, if we allow time, nature usually heals the small scars anyway. Look at New Zealand, particularly the Coromandel Peninsula which was intensively mined and logged; now it is covered with secondary growth and stark pine plantations. Remember that mining scars are infinitesimally small when compared to urban sprawl or clearing of land for farming and grazing, or highways, or the area of most national parks.Thus, miners are important citizens economically, and we are the majority of the few who actually practice the principles of multiple land use.What are the consequences of our image? They are serious in that the poor image we seem to project, discourages many people from becoming involved in, or supportive of, our industry. This brings me to my theme for the year: Students, Education and Communication - the Key to our Future.

Jan 1, 1987

By Harry A. Lipsitt, Douglas Y. Wang

A fatigue study in completely reversed axial tension-compression has been perforried on high-purity titanium and on three high-purity alloys of titanium. The alloys each contain approxi7nately 0.75 at. pct of a single interstitial element; carbon, nitrogen, and oxygen, respectivley. The results corroborate a previously published theory which proposed that strain aging under alternating stress was responsible for the fatigue limit behavior of certain alloys. The present data indicate that in these alloys an increasing strain-talline aging effect under alternating stress is provided by oxygen, carbon, and nitrogen, respectively. CURRENT research on the nature of the fatigue limit in metals suggests that the presence of a fatigue limit in metallic materials is a manifestation of strain aging that occurs under alternating stress.lm5 A comprehensive theoretical model based on the above hypothesis has been developed to explain the existence of a fatigue limit.' This model also provides increased insight into several other fatigue phenomena as under stressing, overstressing, and coaxing effects. The theory, as well, provides equal understanding for those cases where no real fatigue limit is observed. Briefly, this theory assumes that the S-N curve for a pure metal is a smooth function of the applied stress, and the effect of adding an element that is soluble (or forms a precipitate) in the pure metal is simply to shift the S-N curve to the right. If the added element confers the power to strain age, the result is a further shift of the S-N curve, this time upward and to the right. Since strain aging is not expected to be a strong function of stress, and since damage per cycle is known to be quite stress dependent, it is to be expected that there will be some limiting lower stress at which the strengthening due to strain aging will balance the damage due to crack propagation. This stress is the fatigue limit. The position of the fatigue-limit knee was thought to be a function of the magnitude of the strain-aging effect on both the finite and infinite life portions of the S-N curve. Although the strain aging hypothesis seems to be reasonably valid for bcc materials,2'6 it needed to be tested for both fcc and cph metals. This report is the first of a series concerning the fatigue-limit behavior of titanium with varying amounts of the interstitial solutes (C, N,, and 4) that are known to cause static strain aging in titanium. Yield-point effects have been reported for polycrys-talline high-purity titanium alloys containing either carbon, nitrogen, or oxygen.7'9 These effects were observed at testing temperatures in the range 100 to 300'. In addition yield-point and strain-aging effects have been reported for single crystals of titanium containing 0.1 wt pct C plus N.' These yield points were observed over a wide temperature range, but no room-temperature aging occurred. Aging at 180' was required to cause the return of the yield point. The magnitude of the yield phenomena in titanium containing interstitials is not expected to be as large as is observed in bcc metals because of several factors. Titanium has a very high chemical affinity for oxygen and nitrogen. The thermodynamic stability of solutions of oxygen or nitrogen in titanium is recognized. Lattice parameter measurements of titanium containing arbon, oxygen,1° or nitrogen" show that the "c" parameter is expanded more than the "a" parameter, but that up to about 2 wt pct this results in an insignificant change of the axial ratio 'c/a." Ehrlich" has shown that the sites occupied by interstitial atoms in titanium are spherically symmetrical and therefore a lattice expansion, at a constant c/a ratio, results in a simple dilation of the interstitial site. Such a dilation involving no shear has been shown to react only with edge components of dislocations.13 This causes only a weak pinning action. Shear stresses would be anticipated locally when only one of the two interstitial positions was occupied. The carbon atom will cause a symmetrical distortion of the lattice whereas the oxygen and nitrogen atoms have, in addition, the previously mentioned chemical affinity of titanium for these elements. These factors will result in a considerably smaller reduction of free energy upon the association of interstitial atoms with dislocations, and therefore a much weaker pinning than has been observed for the bcc metals. These considerations would lead to the hypothesis that of the interstitial elements considered here carbon would cause the strongest pinning effect in titanium where the amount of interstitial in solution is constant. This hypothesis will be borne out in the analysis of the present results.

Jan 1, 1962

By A. Diaz, Minera Los Pelambres, C. G. Salinas, G. Leinenweber, F. Diaz, D. Rojas, R. Bernal, O. Jimenez

"Los Pelambres Mine (MLP) is located in the IV Region of Chile, a semi-arid region where water plays a key role in operations as a scarce resource and is vital for the sustainability of human life, animals and ecosystem. The conventional flow meters installed on pipes at MLP can fail to provide an accurate measurement due to corrosion and/or fouling on the inner wall or presence of elements in the water such as acids, salts and suspended solids. Conventional flow measurement methods require the inner diameter to be known, however it is not always possible to assess its real value due to scaling, fouling, corrosion, etc. Here we present a novel methodology to solve these problems, which consists of the measurement of flow by a method that does not require the internal area of the pipes: the fluorescent tracer dilution method. In addition, the fluid velocity can be determined by the transit time of a radioactive tracer method. With the flow rate and velocity, the equivalent area is determined and thus the equivalent internal pipe diameter as well. This methodology was applied in a recirculation pump station, for mineral processing from the El Mauro tailings dam.This work demonstrated adequate correlation between measurements from fluorescent tracers and velocity measurements from radioactive tracers, both of which lead to the assessment of the internal diameter of pipes with scaling. The results of both methods disagree with the data provided by the flowmeter installed on the line due to its miscalibration. This information is useful in validating and correcting the information provided by online flowmeters of all water and solutions transport processes in filled pipes.INTRODUCTIONPresently, the need to optimize water resources is increasingly ever important, due to various reasons such as water scarcity, community empowerment, an increased use of water for mining processes and environmental considerations. Taking into account those main considerations, Los Pelambres Mine decided to focus on water conservation to avoid losses of this vital element. They decided to demonstrate that all of the systems that used water (flow meters, pipes, pumping stations, lagoons, etc) were in good condition and that no evitable loses of this important resource occurred. A plan was proposed to conduct a “hydraulic assessment” of fluid flux and water speed at different points and courses at the mine, with the purpose of obtaining hard data to support, verify and correct the information provided online from specific instrumentation dedicated to those purposes. The final goal was to manage the water resource basin in a sustainable way, based on cross-checked information. The chosen points are representative of the processes present in the mine, such as recirculating water stations at different operating conditions and surface water courses, where the fresh water capture systems operate."

Jan 1, 2016

By Jerome J. English, Gordon W. Powell

An experimental investigation and mathematical analysis of the thermal-dilation behavior of the titanium alloy Ti-7Al-3Cb have shown that the linear dimensional changes associated with the polymorphic transformation need not be isotropic. The absolute magnitude of the linear dimensional change, which may be either positiue or negative, associated with the cr-p transformation is dependent upon the relutzve volumes of different orientations of the transformation product. It is hypothesized that the dilation irregulati-ties that have been observed during the polymorphic transformation of pure, coarse-grained titanium and other titanium-base alloys can be explained in the same manner. When titanium is heated above about 165O°F, the hcp a structure transforms to bcc 0. Thermal-dilatioh measurements have shown that the transformation is accompanied by a decrease in length of 0.16 pct.' Such dilation behavior would be expected because the volume of the hcp unit cell is about 0.3 to 0.4 pct greater than that of the bcc unit cell. A recent investigation2 of the thermal-dilation behavior of an experimental a-p* titanium alloy, Ti- 7A1-3Cb, containing 0.06 wt pct 0 showed that its dilation behavior during the polymorphic transformation differed substantially from that reported for unalloyed titanium. The first time the alloy was cycled through the transformation, the dilation curve closely duplicated that of unalloyed titanium. However, upon repeated cycling through the transformation temperature range, both the magnitude and the sign of the dimensional change associated with the transformation were observed to vary with each cycle. This investigation was undertaken to obtain additional data on the dimensional changes associated with the polymorphic transformation in the Ti-7A1-3Cb alloy and to determine the cause of the dimensional irregularities. After testing, the specimens were examined metallo-graphically. In addition, Laue back-reflection patterns were obtained from selected sections taken perpendicular to the specimen axes to determine the a orientations present in these sections. White radiation from a tungsten target and a 0.1-mm-diam collimator were used to produce the diffraction patterns. RESULTS Dilation Curves. Three types of thermal-dilation curves were obtained when the a-8 titanium alloy was heated and cooled through the transformation temperature range. These three types of curves are illustrated in Fig. 1. The type I curve represents what is considered normal behavior, because the dilation change is what would be expected on the basis of the volumes of the unit cells of a and p. The Type I1 curve is the inverse of Type I. Normal behavior is characterized by an expansion on cooling through the transformation, whereas a contraction takes place in the Type 11 curve. With Type ni behavior, no clearly distinguishable length change occurs during the transformation. No other anomalies that might be indicative of other phase transformations were observed in the dilation curves at lower temperatures. Apparently, the cooling rate was low enough for equilibrium to be reached during the 0 to a transformation. Table I lists the types of dilation curves observed during the polymorphic transformation as a function of the direction of measurement and cycle number. The A1 value was determined by extrapolating the low-temperature (a + 5 pct p) and high-temperature (100 pct p) segments of the dilation curves to a common temperature and measuring the difference in the or-dinates at that temperature, see Fig. 1. The transformation occurs over a temperature range in this alloy, so the magnitude of A1 is not an absolute value but depends on the choice of temperature. A mean temperature, T,, within the transformation temperature range was selected for the measurement. T, on cooling occurred about 100°C lower than T, on heating. The first time each of the three dilation specimens was heated to above the temperature, that is, Cycle 2, normal Type I behavior was observed. In Cycle 3, two deviations from normal behavior occurred. First, during cooling of the longitudinal specimen, a substantially larger expansion, +0.21 pct, was measured as 0 transformed to a compared with +0.03 pct in Cycle 2. Second, the thickness specimen was observed to undergo a contraction instead of the anticipated expansion on cooling. Continued cycling of the three specimens from room temperature to 2500°F produced additional changes in the dilation behavior. These changes did not seem to be related to the fabrication direction of the alloy because the values of a1 for the longitudinal, transverse, and thickness specimens varied unpredictably in magnitude and sign. Furthermore, both the longitudinal and transverse specimens showed all three types of dilation curves at least once during the six cycles that they received. Fig. 2 is a sketch of the transverse specimen after

Jan 1, 1967

By D. T. Goettge, E. L. Robinson

The phase changes occurring in low carbon steel during hot strip mill rolling are shown to be metallurgically significant when related to commonly used temperature control points, particularly finishing and coiling temperatures. In combination, these temperatures are shown to have an important influence on the level and uniformity of hardness, grain size, and carbide characteristics of the finished hot and cold rolled sheets. PRODUCTION of wide flat-rolled products ordinarily requires a number of operations in sequence to prepare the material for shipment to the customer. Most products are tailor-made for specific end uses, with each operation contributing certain properties to the finished material. Since the characteristics imparted to the semifinished product by a given step in processing carry through to the finished product in varying degrees, it is important that the intermediate stages of production of flat-rolled strip be carried out with the same care which characterizes the last or finishing operations. The step of hot strip mill rolling is common to the production of all of the various types of flat-rolled product; therefore, the hot strip rolling is an especially important point at which to recognize and control those variables which have an effect on the surface characteristics and metallurgical properties of the finished product and which influence the ease of conducting subsequent operations. Orders entered at a producing mill usually show an end use or describe an article or part into which the ordered product is to be fabricated. Applying his experience as to the properties necessary in a finished sheet to suit the end use and to perform successfully in the fabrication involved, the metallurgist selects a steel of suitable composition and deoxidation practice, and slabs of appropriate dimensions are produced for rolling on the hot strip mill. At this stage of processing, the metallurgist faces the problem of controlling hot strip mill practice in the light of his diagnosis of the properties necessary to meet the end use, paying due attention to the accompanying problem of producing a strip which can meet processing requirements on subsequent units in the mill. It is the purpose of this paper to describe some of the factors which he must consider in solving these problems and to indicate some of the principles which guide him. Equipment, Physical Requirements of the Strip, and Temperature Measurement The metallurgist must, of course, be familiar with the physical layout of the mill, the temperature-measuring equipment available, and the physical requirements of the hot strip product before he can apply his metallurgical knowledge to the problem; hence, the first section will consist of a brief discussion of these matters. The usual hot strip mill consists of reheating furnaces, five or six roughing stands including a scale-breaker, holding table, and second scalebreaker, six-stand finishing mill, runout table with spray cooling facilities, and coilers. A schematic diagram of a typical layout is shown in Fig. 1. Slab temperatures are primarily a function of heating time and furnace temperatures, while mill speeds, spray practice, drafting practice, available water pressure, temperature of the cooling water, cross sectional dimensions of the strip, coil size, and equipment limitations, either singly or in combination, determine what rolling temperatures are practical on a given hot strip mill unit. Thus, it is possible that a set of temperatures which can be utilized successfully on one mill cannot be used on another. However, adjustments in temperatures and rolling practice can usually be made to develop the desired metallurgical properties. In addition to the metallurgical properties developed through proper temperature control, the hot strip mill must also provide strip with certain physical attributes which may be summarized as follows: Strip Cross Section—The strip contour should conform to a section which will give the best results in the cold reduction operation. This is generally recognized as a strip with 0.001 to 0.003 in. crown or shoulder-to-shoulder convexity depending on width, and freedom from concave, flat, or wedge-shaped cross sections which cause metal buildup in cold reduction. Excessive drop off in thickness at the edges can also be very detrimental in cold reducing to light gages. Gage, Width, and Camber—All of these must be controlled. For example, rundown or increasing thickness from the front to the back of the coil results in nonuniformity in the thickness of hot-rolled sheet product and in added difficulty with gage and welds in cold reduction. Similarly, excessive width variation is the cause of guide trouble and excessive edge scrap at later stages of processing, while excessive camber is the source of a variety of processing troubles. Type of Oxide—Product intended for pickling should have a predominance of the type of oxide most easily removable in sulfuric acid. It is generally recognized that this type is obtained by use of maximum table cooling water and cold coiling

Jan 1, 1957

By Eli T. Conner

My connection, under a commission from the Councils and Board of School Control of the city of Scranton, Pa., with a recent investigation of mine-caves and the resultant damages to surface-improvements, has led to the preparation, at the invitation of our Secretary, of the present paper. It is notorious that there are, in the anthracite-fields, frequent subsidences of the surface, due to the removal of the coal beneath. No particular attention is paid to such occurrences, unless they happen to injure surface-improvements. Many caves have happened in Scranton and its viciuity, which hare excited but little remark, since they have generally caused no serious damage. In August, 1909, a cave occurred in the Hyde Park section of the city, generally known as the West Side, which nearly destroyed school-house No. 16 and considerable adjacent property. Fortunately, there were no pupils in the building at the time; but the thought of the possible result, had the usual number of pupils and teachers been present, aroused the public to the gravity of the situation; and the School Board employed engineers to investigate the case. Two reports were made by separate sets of engineers, which differed in some particulars. These differences were pointed out in the public press and magnified, and the consequent agitation of the subject was taken up and greatly exaggerated by some of the metropolitan newspapers, giving to uninformed people the very erroneous impression that the whole city of Scranton was in danger of sinking into the bowels of the earth. All this tended to affect the credit of the city and to depress real-estate values. The matter was considered at a joint meeting of the Board of Trade, the Councils, and the School Board. The Hon. J. Ben. Dimmick, a former Mayor, suggested that it

Jan 1, 1912

By A. S. Yue, A. G. Guy

A study was made of the effects of a prolonged flux of zinc atoms through the a solid solution of zinc in copper. The experimental arrangement consisted essentially of a copper disk about 0.01 in. thick, at one of whose surfaces a gaseous atmosphere containing zinc atoms was maintained, and at the other surface a gaseous atmosphere with a minimum of zinc atoms was maintained. During prolonged theothersurfaceexposure at high temperatures the zinc content of the copper disk gradually built up to the steady-state concentration distribution and then remained at this value. The concentration-distribution curves for various conditions were determined by chemical analyses. The results showed that the condition of steady-state diffusion was achieved. The diffusion coefficients calculated from the experimental data, although not of high precision, agreed with the values obtained by other workers using unsteady-state methods. Relatively slight porosity developed in the specimens in the course of diffusion. A LTHOUGH most diffusion studies have been made under unsteady-state conditions, it is known' that the steady-state method is often superior with respect to the directness and accuracy of interpretation of the data. Steady-state diffusion of gases through metal diaphragms is well known. Also, Harris' and Smith" have used the steady-state method in studying the diffusion of carbon in aus-tenite. The accepted mechanism in this system involves the motion of the interstitial carbon atoms in the rigid framework of the lattice of iron atoms. Thus, there is little difficulty in visualizing the steady flow of the small carbon atoms through the austenite. The situation in substitutional diffusion is quite different. Here the atoms are comparable in size, and it is not evident how a steady flow of one of the atoms through the solid solution might be achieved. At the time the present research was started, it was known that a previous exploratory attempt to produce steady-state diffusion in a substitutional alloy, the Au-Ag system,' had been unsuccessful and had indicated that perhaps there were basic difficulties that could not be ovei-come. Therefore, the present research began as a study of the effect of a prolonged flux of metal atoms through a substitutional solid solution. Eventua.lly, it was possible to produce actual steady-state diffusion in the system chosen for study, the a Cu-Zn alloys. Experimental Procedure The aim in the experiments was to maintain a high zinc content, about 30 pet, at one surface of a copper sheet, and to maintain a low zinc content, near 0 pet, at the opposite surface. The zinc would then diffuse into and through the copper, first building up to the steady-state concentration distribution and then maintaining this distribution. The three types of specimens that were used are shown in Fig. 1. In type A specimens the copper disk through which diffusion occurred was welded to the top of a cylindrical molybdenum tube, the bottom of which also was sealed by welding. At the diffusion temperature the brass chips in the molybdenum container were the source of the zinc vapor which maintained the lower surface of the copper disk at 30 pet Zn. The upper surface was maintained at 0 pet Zn by the vacuum in which type A, and also type B, specimens were diffused. Since the molybdenum container was impervious to zinc vapor, it was intended that the only path of escape for the vapor from the brass chips would be through the thin copper diffusion disk. However, it was found that small leaks often developed at the welded joints during the diffusion treatment, and in most specimens some of the zinc was lost in this manner. Although even small losses of this kind were a serious handicap in attempting to determine the flux through the disk, they did not prevent the maintenance of satisfactory boundary conditions for the attainment of the steady-state condition. Type B specimens differed from type A in having a weight of about 300 g supported on the copper disk by 15 to 20 short quartz rods. This change was made when it was observed that the copper disk was being bowed upward by the difference in the pressures acting on its two surfaces. Since the grain-boundary cracking which occurred in the bowed specimens could be attributed largely to the accompanying creep,3 it was desirable to minimize this effect. The counterweight was effective in significantly decreasing both bowing of the disk and cracking at grain boundaries. Type C specimens differed considerably from the others in that the low-zinc atmosphere at one sur-

Jan 1, 1959

By C. Alan Tapp

Introduction Mine sampling determines the practicality of any mining operation. Improper sampling can result in an incorrect appraisal of present production and future potential. Therefore, the mine department in charge of ore-reserve calculations and mine sampling should be overseen by competent and experienced professionals with technical backgrounds qualifying them to produce accurate results. Sampling is a process by which portions of an ore body are collected and analyzed to estimate the average mineral content of the entire ore body. It is incorrect to assume that a large number of samples eliminates any errors in the sampling method. To obtain unbiased samples, proper sample location with respect to rock type and mineralization is just as important. The sampling procedure must yield correct results for the type of mineral deposit, and careful consideration should be given to whether or not the sampling technique has been developed to an extent sufficient to eliminate as much human error and bias as possible. Only after the ore has been mined and milled is the sampling accuracy known. Sampling also provides information about the bulk composition of the ore for mineralogical and metallurgical tests that determine the economic ore-waste boundaries and the geologic trends for exploration. Actual mining plans can be developed from this information to maximize profits. Accurate sampling is critical, and thus must be approached in a scientific manner. Sampling Techniques Sampling practices and techniques are as varied as the mines in which they are used. The method(s) chosen must be tailored to suit the company and mining needs. For instance, tabular uranium deposits, vein gold deposits, and porphyry copper deposits pose special problems in conducting unbiased sampling. The mine geologist or engineer in charge must develop a sampling method, test it in a sample area, and then critically evaluate the results. If the results from the test area are accurate within the economic limits established by the company, they then may be adopted for general use in the mine. Four routine sampling methods are suitable for specific sampling objectives in the daily mine routine: (1) channel sampling, (2) chip sampling, (3) grab sampling, and (4) bulk sampling. The final sampling results depend upon how the four methods are combined to accurately determine the grade of the ore body. When used in conjunction with each other during different stages of mine development, the channel, chip, grab, and bulk sampling methods provide an in-house check or a comparison by which mining methods and sampling procedures can be evaluated. However, the most valid check is based upon the daily mill production. Channel Sampling Channel samples consist of cuttings collected from a groove cut into the rock about 102 mm (4 in.) wide and 19 mm (0.75 in.) deep. Various tools ranging from a 1.8-kg (4-lb) hammer and moil to a pneumatic chisel can be used to cut the sample. Accessibility and rock hardness determine the applicable sampling tools. Before attempting to take a sample, the rock surface must be cleaned thoroughly; the method of cleaning depends upon the amount of mine dust accumulated on the surface or the degree of alteration of the rock surface. Typical cleaning methods 'employ a wire brush, water, or chipping a fresh surface. Next, the sample outline is marked on the prepared surface, taking care to choose appropriate sample loca- tions. After determining the proper sample outline and length, the sample can be chiseled out, catching the rock fragments on a canvas tarpaulin on the floor, in a powder box, in a canvas bag to avoid contamination, or by some other suitable means to capture all of the sample. Vertical veins present a special problem because the drift's back usually is arched, not square. For example, Fig. 1 shows that if sample intervals are measured from A' to D', the length of the sample interval is greater than the true vein width, resulting in an incorrect calculation of the ore reserves. The correct method would collect three samples at A'-B', B'-C', and C'-D', using either actual measurements in the mine represented by A-B, B-C, and C-D or trigonometric calculations to determine the true ore thickness. Then, each sample can be weighted by grade and true thickness for the vein. Channel lengths usually are a maximum of 1.5 m (5 ft), and it is good practice to divide longer samples into smaller intervals according to structures, changes in rock types, or differences in rock hardnesses. The influence of those features on the mineralization then can be determined. Chip Sampling Chip sampling is a variation of channel sampling used when the rock is too hard to channel sample economically or when little variation in the mineral content indicates that this sampling method will yield results similar to those of channel sampling. Rather than cutting a channel in the rock, small chips are flaked off at regular intervals over the entire face or area being the mine. sampled. Care must be taken to assure that the sample is representative of variations in the rock hardness and type. hi^ method is fast and useful in preliminary evaluations, but it should not be used for quantitative ore-reserve calculations. Grab Sampling Grab sampling is a fast method for double checking either channel or chip-sampling procedures, and, in some instances, mine production can be estimated from carefully taken grab samples. Grab sampling takes equal amounts of material at selected intervals over a mine dump, a muck pile, or from an ore car to estimate its Channel Sampling mineral content. Generally, this method is not considered reliable. Many independent variables can affect this type of sampling process. Thus, if the ore occurs in the softer fraction and a proportional amount of the result-

Jan 1, 1982

By E. R. Haymaker, C. W. Binckley, F. R. Burgess

A method of establishing stabilized back-pressure curves for gas wells producing from formations of extremely low permeability is presented. Actual well performance under many different operating conditions is shown by the stabilized back-pressure curve. By use of the method. it is possible to conduct back-pressure tests with a critical-flow prover on wells that stabilize slowly, and save approximately 88% of the gas ordinarily vented to obtain satisfactory test data, with a great reduction in time required for testing. INTRODUCTION The reasons for establishing dependable back-pressure curves on gas wells have been pointed out by previous publications. The publication most referred to. of course, is the United States Bureau of Mines Monograph 7, titled "Back-Pressure Data on Natural Gas Wells and Their Application to Production Practices". The technique generally established therein has been accepted and used by many engineers; and, when proper tests are conducted, the results can be used for the analysis and solution of several practical problems concerning field operation and development. Even where formations of low specific permeability are encountered, the determination of a well's actual performance by the back-pressure test method permits the engineer to analyze many problems in individual well operation and also to predict necessary future field development. Such problems as the determination of the ability of a well to produce into a pipe line at a predetermined line pressure, the design of gas gathering systems and meter settings, and the determination of the time and the number of wells required to be drilled to meet future market obligations, can be solved, in part., by the use of a reliable back-~ressure curve. In addition, the computed well delivery rates determined by data from backpressure tests ordered by state regtilatory bodies, when compared with the true back-Pressure curve, permit the operator to ascertain whether such data represent unstable or relatively stabilized delivery rates for given pressure conditions of the well. The technique of back-pressure testing, as described in this report, was developed by Phillips Petroleum Company engineers from data obtained during a testing program that started in 1944 and has been continued to date. Three hundred and eleven back-pressure tests were conducted on 299 wells located in the southern part of the Hugoton Field. The gas-bearing zone is composed of several dolomitic formations of the Permian Age; the important ones are the Herington, Upper Krider, Lower Krider, and Winfield. The average bottom-hole temperature is approximately 91 °F.. and the initial wellhead shut-in pressures range from 400 to 440 psig. The spacing pattern is 640 acres per well with each well located near the center of the section. The range of back-pressure potentials on wells tested was from 500 to 23,000 Mcfd. All gas wells were acidized, and the quantity of acid used, expressed in 1574 hydrocloric acid, varied from 12,000 to 22,000 gallons per well. The quantity and concentration of each treatment depended on the stage, the formation being treated, and experience gained from previously completed wells. The gas in the Hugoton Feld is a "dry" gas. It has a gasoline content of approximately 0.25 gallons per thousand cubic feet, as determined by charcoal test, and its specific gravity averages about 0.71 as compared to air (air = 1.00 at 60°F.). Of the wells tested, 71 were completed with 7" casing, 3 with 9 5/8" casing, and 1 with 6%" casing set on top of the upper producing formation with the well bore through the gas bearing formations being open hole. Two hundred and twenty-four were completed with 5 1/2'' O.D. casing set through the gas bearing formations and perforated. For the purpose of establishing reliable back-pressure curves in the area, Phillips Petroleum Company personnel has computed data on the basis of 24-hour flows per point. Early in the program, many tests were actually permitted to flow 24 hours to obtain data for each plotting point, at great expense in man power and time. Presently, however, such tests have been replaced by tests of short duration flows which can be made to effect results that correspond to the tests obtained by flows of much longer duration. METHOD When a gas well producing from a reservoir of low permeability is opened for production through a constant size orifice, both the rate of flow and working pressure decline. first at a high rate and later at a lower rate until after several hours the decline becomes difficult to ascertain. In this paper the rae of flow and working pressure are considered to be stabilized when it becomes difficult to observe changes in working pressure during a period of three hours by the use of a deadweight pressure gage. Stalibization of pressure in the literal sense is never obtained in a producing gas well. In formations of low permeability. such as those in the Hugo-ton Field, most wellhead working pressures approach stabilization closely enough to be used satisfactorily in the determination of a back-Pressure potential curve after flow periods of 24 hours. We shall therefore describe the backpressure curve calculated from ohserved rates of flow and working pressure at the end of 24-hour flow periods.

Jan 1, 1949

By B. E. Eakin, R. T. Ellington

An apparatus and a procedure for determining the viscosity behavior of hydrocarbons at pressures up to 10,000 psia and temperatures between 77 and 400° F are described. The equipment is suitable for measuring viscosity of either the liquid or vapor phases or the fluid above the two-phase envelope for systems exhihiting retrograde phenomena, according no the phase state of the system within these ranges of temperature and pressure. Equations are developed for calculation of viscosity from the experimental measurements, and new data for the viscosities of ethane and propane at 77° F are reported. INTRODUCTION With the advent of higher pressures and temperatures in industrial processes and deep petroleum and natural gas reservoirs, demand has increased for accurate values of physical properties of hydrocarbons under these conditions. Proportionately, more frequent occurrence of natural gas and condensate-type fluids is encountered as fluid hydrocarbons are discovered at greater depths. This increases the importance, to the reservoir engineer, of being able to predict accurately the physical properties of light hydrocarbon systems in the dense-gas and light-liquid phase states. Reliable gas viscosity data are limited primarily to measurements made on pure components near ambient temperature and at low pressures. Few investigations have been reported for high pressures, and except for methane, data on light hydrocarbons are subject to question. This is demonstrated by the large discrepancy between sets of data on the same component reported by different investigators. For mixtures in the dense gas and light liquid regions and for fluids exhibiting retrograde behavior there are very few published experimental data. Viscosity data for methane have been reported by Bicher and Katz,1 Sage and Lacey,12 Comings, et al,3 Golubev,3 and Carr,3 with good agreement among the last three sets of data. Comings, Golubev and Carr utilized capillary tube instruments for which the theory of fluid flow is well established. The theory permits calculation of the viscosity directly from the experi- mental data and dimensions of the instrument alone. Sage and Lacey, and Bicher and Katz used rolling-ball viscometers. The theory of the rolling-ball viscometer has not been completely established, and these instruments presently require calibration by use of fluids of known viscosity behavior before viscosities of test fluids can be measured. To obtain accurate data it is necessary that the rolling-ball viscometers be calibrated by use of fluids of density and viscosity similar to the test fluids, a difficult selection for the gas phase. From the methane data and experimental tests on various natural gases, Carr developed a correlation for predicting the PVT behavior of light natural gases.2,3,4 This correlation was based on data for a very limited composition range; its application to rich gases and condensate fluids is questionable. The object of this investigation is to develop an instrument which can be used to obtain viscosity data at reservoir temperatures and pressures, for rich gases, condensate-type systems above the two-phase envelope and light liquid mixtures. These data will be used in an effort to develop correlations to represent the viscosity behavior of these fluids. APPARATUS In a previous viscosity study Carr2 utilized a modified Rankine capillary viscometer configuration," Fig. 1. In this instrument the gas to be tested is forced through the capillary tube in laminar flow by motion of a mercury pellet in the fall tube, the measured displacement time being that required for the mercury slug to move between the brass timer rings. The viscometer is constructed of glass and mounted in a steel pressure vessel. The test gas pressure in the viscometer is balanced by an inert gas (usually nitrogen) in the vessel. Excellent results have been obtained with instruments of this type, with Carr2 and Comings5 reporting repro-ducibilities of 99.5 to 99.3 per cent and an estimated absolute accuracy of 99 per cent. However, these instruments have limitations which have precluded their use for liquids. The need for maintaining a balance between pressures of the test fluid and inert gas in the viscometer vessel presents operating problems, and requires charging the test fluid to the viscometer very slowly. The principle drawback to the Rankine unit is behavior of the mercury slug which provides the pressure differential across the capillary. When even trace quantities of propane or heavier hydrocarbons are present in the test gas, the mercury tends to subdivide

By Lloyd M. Kniffin

[This paper is one of series being prepared by the United States Bureau of Mines on mining methods, practices, and costs in the various mining districts of the United States. It describes the mine of the Hanover Bessemer Iron & Copper Co. at Fierro, Grant County, N. M., which is the only operating iron mine in the southwestern part of the United States. This mine is in a district noted for the great variety of ores that it produces. Within a small area, as shown is Figure 1, there are noteworthy deposits of nearly all the common metals. The ore occurs in lenticular masses dipping at about 50°. An underhand stoping method has been developed that requires but a very small amount of handling of ore. As the ore is very irregular in iron content and also in the distribution of the impurities--chiefly sulphur, silica, and magnesia--a method has to be used that will permit selective mining and will also allow ore and waste to be taken out separately as conditions change. A magnetic cobbing plant raises the grade of the ore shipped about 10 per cent.]

Jan 1, 1930

By Bernard M. Larsen, Clyde F. Williams, Edward P. Barrett

"Introduction.The Bureau of Mines at its Northwest Experiment station has been studying the production of sponge iron for the past four years, and during 1923 progress advanced to the point industrial applications can be safely considered. A furnace was operated commercially at silver City, Utah, producing about three tons of sponge iron daily.The Bureau was led to undertake this work by the interest in the use of sponge iron for copper precipitation and for conversion to iron and steel in the electric furnace.If a piece of iron oxide is completely reduced at such a low temperature (850 to 900° C) that no sintering or fusion takes place, then the piece of metallic iron formed has the same size and shape as the original piece of oxide on account of the removal of oxygen, the structure is finely porous, exposing a large surface of iron, and the apparent density is less than that of the original piece of iron oxide. This material is called ""sponge iron"". Chemically, it is a very reactive material."

Nov 1, 1924

By Arno C. Fieldner

In view of the widespread interest in the production of synthetic liquid fuels from solid and gaseous fuels to supplement declining reserves of petroleum, and the many requests that are now being received for information on the subject, this bibliography of Bureau of Mines contributions has been compiled. In addition to the publications issued by the Government in printed or mimeographed form, references are included to articles written by the Bureau staff for the technical press and to cooperative reports of work done jointly with States, colleges, and industries. References are given under each section in chronological order. Bureau of Mines bulletins, technical papers, and Minerals Yearbooks are printed and are obtainable at the prices indicated from the Superintendent of Documents, Government Printing Office, Washington 25, D. C. If no price is given, the publication is out of print. The price of entire volumes of the Minerals Yearbook or of reprints of certain chanters may be obtained upon request. Any orders or remittances in payment for these publications should be cent directly to the Superintendent of Documents and not

Jan 1, 1945

By Robert L. Zook

Coal refuse slurry impoundments are dams constructed of coarse coal refuse to impound fine refuse (slurry) and water (25-30% solids). Both products are waste from coal preparation plants. A number of these structures in West Virginia, Pennsylvania and Kentucky were investigated to determine embankment stability. During the investigation a variety of embankment designs were encountered. The investigation determined the soil and geological characteristics of the embankments and the sites. This was accomplished by a test drilling and monitor installation (observation wells and piezometers) program, geologic study, and large scale mapping which allowed sub-surface profiles of the embankments to be constructed. The laboratory testing program concentrated on textural classification of the coal refuse, permeability and determining strength parameters to be utilized in the stability analyses. For the stability analyses, the Modified Fellinius Slip Circle, Simplified Bishop Slip Circle and Analysis for Translational Failure -were utilized. In all stability analyses hydrostatic pressure and earthquake were considered. This investigation indicated that 62% of the embankments analyzed are in a stable condition. The coal seam mined, the type of roof rock, and the gradation of the refuse influence the degree of compaction obtainable and the permeability of refuse. The shear strength of coal refuse appears to be controlled by its composition, moisture content, degree of compaction, amount and grain size of fines present. This investigation demonstrated these em¬bankments should not be treated as pure state-of-the-art dams; consideration must be given to the particular properties of coal refuse and the total refuse disposal system. Refuse dim slurry impoundments generally lack the site se- lection phase that is standard practice with siting most other types of dams.

Jan 1, 1974

By E. W. Sawyer

Gelling-grade attapulgite and sepiolite clays are employed as thickening agents for the preparation of ionically contaminated drilling fluids where the use of fresh water clays are unfeasible or impossible. Attapulgite and sepiolite are nonswelling clays that can be dispersed and reflocculated by mechanical and chemical means to increase the viscosity of fresh water, salt containing waters, gypsum contaminated waters and fluids containing cement. Such gelled systems are quite stable in viscosity properties and can be further treated with other necessary additives such as thinners, water loss reducers, weighting agents, surfactants, etc. Many of the oil well drilling fluid practices have influenced such technologies as water well drilling, foundation drilling and waste disposal. The use of salt water gelling clays in these fields will be described and compared to oil well drilling.

Jan 1, 1986

By K. H. Boss

In modern iron pelletizing plants fuel consumption has been optimized to such an extent that only minor savings can be expected in the future. Inspite of this fact, different process parameters were studied with a mathematical model and firing tests. The influence on fuel consumption and productivity was established. Furthermore, the adoption of simplified firing patterns was investigated, in particular for coal firing. In view of high costs of oil and natural gas, only substitution of these fuels by coal can substantially reduce production costs. In existing plants partial replacement of oil and gas can be achieved by addition of coal to the iron ore feed and by firing the pellets with pulverized coal. Two systems have been developed for the Lurgi- Dravo travelling grate process which enables coal to completely replace oil or gas. This paper describes in the first part the potentials for fuel savings available in the Lurgi-Dravo process. In the second part, different techniques for the use of coal as fuel in iron or pelletizing plants and in particular the recently developed Lurgi Multistage Coal Injection and Combustion Process (LMC) are discussed. Combined with the LMC process, a wide variety of iron ores and coals - also with high ash contents - can be used in the Lurgi-Dravo travelling grate process.

Jan 1, 1983

By R. A. Cattell

Every finding of the year's work, obtained under stress to meet present objectives, contributed to postwar needs, because the very nature and constitution of petroleum and natural gas require that research be conducted along the same general lines whether the results are applied in peace or war. More than 40 reports were submitted to the Petroleum Administration for War and others concerned with (1) evaluation of crude oils to determine their content of aviation-gasoline base stock, (2) evaluation of base stocks for blending with high-octane, synthetically manufactured components, (3) analyses of naphthas to determine their content of various types of hydro-carbons, such as benzene and toluene, and (4) the improvement of quality of marginal base stocks to meet future requirements of aviation gasoline. This upgrading of marginal stocks is being attained by selective distillation and chemical and catalytic removal of sulfur compounds. Asphalts were studied with respect to the characteristics of their various constituents in order to compound them, in the same way that aviation fuels now are being "built" to meet exacting requirements. The work previously initiated to give the industry fundamental data on thermodynamics of hydrocarbons progressed satisfactorily, and the heats of combustion of 10 hydrocarbons in the lubricating oil -range of petroleum were determined. Thermodynamic data requiring highly specialized techniques are so broad in application that their commercial usefulness is not yet fully appreciated.

Jan 1, 1946