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By James R. Stuart

AS the available remaining properties of iron ore reserves on the Mesabi Range are opened up for mining, the various properties located under lake beds are brought nearer an active status. The actual physical problems involved in stripping these properties do not act as a deterrent so much as the legal and political problems that are encountered. When it is proposed to destroy a natural lake that has been used by the public for many years, much local as well as state opposition may be encountered regarding its destruction. Public hearings must be held and some adverse publicity is likely to result. The ownership of the ore under the lake and the rights of the abutting property owners must be settled, and protection from damage caused by a disturbance in surface and subsurface drainage is likely to be demanded by property owners some distance from the proposed mine area. The Embarrass Mine, located near Biwabik, Minn., falls into this classification. A portion of the orebody lies under what was formerly Syracuse Lake, this body of water having been removed in the process of stripping the mine. An additional problem in the case of a meandered body of water is the establishment of a meander line that can be projected downward as mining progresses to form the basis for a satisfactory division between lake bed and upland ore shipments for royalty purposes. Fig. 1 illustrates the complications encountered in maintaining these divisions. A balance point was agreed upon in the center of the lake to make an equable division of lake bed ore to the abutting properties. The entire lake bed has since been adjudged the property of Minnesota. Lake Characteristics Lake bed stripping problems with which this paper is concerned necessarily are limited to a specific type of lake, namely the glacial lakes of the Lake Superior region. One characteristic common to these bodies of water is a deposit of fine black mud or silt on the bottom, frequently underlain by a layer of impervious blue clay. This is also true of the muskeg areas of the region, which present almost identical problems as lakes in stripping. The actual removal of the water and the lake bed material is a routine matter more or less standardized as to equipment, and the period of time required can be estimated easily on the basis of volume and capacity. More important than the foregoing is the execution of preliminary work, and above all, the timing involved. An account could be prepared based entirely on statistical and cost data which would give a very fair picture of the time required and cash outlay needed to effect the removal of a body of water preliminary to stripping the orebody. However, the real interest from the standpoint of the operator and the engineer who carry responsibility for completion of the job lies in the unexpected emergencies and the action of various materials involved in the stripping when the balance has been upset through diversion of water courses and the reduction of the lake level. Runoff and Drainage Lakes are located in natural basins that catch all the rain water and runoff water for a considerable area. Where a lake is involved having an inlet and outlet or a sizeable water course running through it, the drainage area may include a watershed covering many square miles. All available data then must be collected to supply a history extending over as many years for which information can be gathered on the flow of streams, annual rain and snowfall, and most important, the peak flows to be expected. Where the diversion of a stream around the stripping area is a part of the problem, this last factor is of great importance since it controls the cross-section to be selected for the diversion channel and the volume to be removed in its excavation, as well as affecting the hydraulic considerations to be met in the design of the completed channel. Characteristic material in the overburden found at the Embarrass Mine is illustrated in Fig. 2. Well Pumping Pumping from the well holes was started well in advance of the draining of the lake. Fig. 3 shows a gradual lowering of the water table with no noticeable fluctuations during the period in which the lake was being dewatered. Unfortunately, because of tight ground, a maximum flow to the wells was not maintained. This retarded the rate at which the water table was reduced so that in the course of stripping the excavation soon extended below the water table, and the great bulk of the pumping was handled from a system of sumps in the pit itself. Any dewatering program projected by prepumping from wells, a glorified well point system, would have to be started well in advance of the stripping to be of any great advantage. Preliminary drainage of the surface over the mine area is entirely apart from the actual elimination of the lake bed itself. Since the lake is what is called a perched water table because of the impervious character of the lake bottom, the adjoining surface may be dewatered below the surface of the existing lake and the flow will not be affected by the proximity of that body of water. This condition actually has been demonstrated through the establishment of a number of observation holes where a small churn drill was used to put down the holes and a 3-in. pipe was installed for taking water level

Jan 1, 1952

By Carl H. Beal

DURING the latter part of 1915 and the first half of 1916, the writer held the position of geologist in connection with the conservation work instituted by the U. S. Bureau of Mines, on oil and gas land belonging to the Indians of the Five Civilized Tribes in Oklahoma. The duty of the geologist was to correlate formations containing oil, gas, and water, and to determine the relations of these substances in the different formations so that the conservation agents might carry on their work most intelligently. On account of the rapid development of the Cushing field, which lies in the western part of the Creek Nation, much work was done there by the inspection force. In the course of the geologic studies a large amount of information was collected, which, on analysis, has disclosed some interesting facts worthy of publication. The report, of which the following remarks are an abstract, has been prepared and submitted to the U. S. Geological Survey for publication. This report is now (June, 1917) in the press and will doubtless be issued in a few weeks. Methods Used In addition to the structure maps showing the folding of the Pawhuska limestone, which crops out in several places in the Cushing field, separate structure maps of the three most important productive sands—the Lay-ton (Fig. 2)) Wheeler, and Bartlesville—have been prepared. These structure maps were prepared by obtaining the logs of nearly all the wells

Jan 1, 1918

By D. A. Dahlstrom

THE necessity for slime elimination from valuable mineral and coal products has become increasingly significant within the past 5 years.1,2 Most of the mechanized mining and present beneficiation methods have resulted in larger tonnages of extreme fines, silts, and clay, commonly called slimes, processed by the preparation plant. Economics in turn have forced the plant operator constantly to lower the bottom size of effective beneficiation, necessitating an almost complete recovery of valuable solids regardless of particle size. When these important factors are considered, the need for an efficient slime removal method for fine solids becomes self-evident. Ordinarily slimes have been classified as ranging from 75 microns, or 200 mesh, down to colloidal dimensions of less than one micron. At the same time there is general agreement that the most troublesome slimes are primarily clays, silts and extreme fines, so that the actual top size may be placed at approximately 30 to 40 microns. This immediately restricts any desliming operation to classification, as screening or other methods would be both uneconomical and grossly inefficient at such dimensions. The liquid-solid cyclone has been recognized as one of the most efficient fine size classifiers available to the mining industry. Applications of cyclones to thickening, high efficiency solid recovery, degritting,

Jan 1, 1952

By W. E. Bearce

The recent concern for the recovery of even the finest fractions of coal preparation plant feeds has created needs for new equipment. Thermal dryers currently available have difficulty reducing the filter cake moisture on down to the desired point. This difficulty involves 1) the physical problem of handling this wet, sticky material and making each particle accessible to the hot gases, and 2) removing the extremely fine dried particles from the cooled gases. The dryer described in this paper handles the first of these problems, and eliminates the second by the substitution of steel balls for air as the heat transfer medium. As a general statement, the cost of preparing coal for market is inversely proportional to the size of the lumps or particles. In the not too distant past the finer sizes were discarded as being uneconomical to treat and this practice might be still continuing if it were not for the insistence of the public that this material be kept out of our streams. This being the only cost-free outlet, the disposal of fine refuse became a significant item of expense in every preparation plant. When this happened it was only reasonable to look to the recovery of the values in this material, not only to defray this expense, but to reduce the tonnage which had to be wasted. There seemed to be no device available suited to reducing the moisture in this material to what the market requires. All of the fine coal dryers commonly employed make use of air to bring the heat of combustion into contact with the coal particles. Any device employing air as a heat transfer medium, has the following two strikes against it in attempting to handle 28 mesh by 0 filter cake: 1) It is practically impossible to bring the hot air into intimate contact with the enormous number of fine particles stuck together in the cake. 2) Even if this can be effected, it is impossible to remove the dried coal from the air. A wet scrubber must be employed, the discharge of which must go back to the filter and dryer as a circulating load of the most objectionable sort, being the extreme fines. Various compromises have been used to cope with the problem of drying this relatively small tonnage of high moisture coal. Often some of the dried coal is mixed back with the feed to the dryer in an attempt to make the mixture more handleable and more available to contact with the hot air than the filter cake alone would be. This may help to some extent with the first problem but it does nothing about the second and a dryer operated in this way has to be oversized. Sometimes the filter cake is mixed with a coarser fraction for the same reason. Here again, while this may make a mixture (the particles of which are more readily brought into contact with the hot air), the problem of getting the fine coal out of the air remains and a larger percentage of the total coal to be dried is handled by the most expensive means. Mechanical dewatering has accounted for more and more of total coal drying lately and in many cases would satisfactorily handle the whole load, down to 28 mesh, if there were a means available for doing a good job on the —28 mesh by itself. The dryer which is the subject of this paper was designed expressly for doing this job — drying fine material by itself regardless of how wet it may be to start with, how fine it may be, or how gummy and sticky these properties in combination may make it. The essential features are depicted in Fig. 1. A rotating cylinder is supported on a frame in such a way that one end may be raised or lowered by hy-

Jan 1, 1968

By D. C. Seidel, E. F. Fitzhugh

Nickel sulfide ores lend themselves readily to concentration before smelting or pressure leaching, but neither of the major oxidized ore types-the iron-rich laterites and magnesium-rich, soft silicates-has been directly concentrated. Upgrading of crude ore in current practice is limited to cobbing lumps of the harder, lower grade rock (protore) from the softer, enriched silicate ore, because only a small percentage of the nickel in these ores occurs in discrete, contrasting mineral particles. There is no apparent mineralogical contrast in the superficial, iron-rich lateritic ores and, in fact, there is no firm assurance that the nickel atoms are within the lattices of the limonite minerals, or else irregularly adsorbed on the limonite. Within underlying, "rotten rock" silicates, occasional veinlets of garnierite and related nickeliferous silicates are found.1 The garnierite veinlets are only incidental, and the majority of the nickel atoms occur as erratic replacements of magnesium atoms in the micaceous chlorites of the ore mass.

Jan 4, 1968

By John J. Porter

The requirements of the standard specifications under which Portland cement is sold have materially increased within the past 10 years, but practically all companies are now furnishing cement better than these requirements; in some cases exceeding them by nearly 100 per cent. From a sales standpoint, it is desirable to have a product that is uniform to a high degree and free from occasional quality troubles. A failure in quality, even if it affects only a few hundred barrels out of a yearly output of a million or more, is apt to be talked about in the trade and to affect the salability of the entire output. For these reasons, there has recently been great activity along the lines of quality control and improvement; and some of the most interesting problems of the industry are in this field. From the manufacturing standpoint, the quality of cement is chiefly a matter of uniform and proper chemical composition of the raw mix fed to the kilns plus proper burning in the kilns; the fineness to which the cement is ground, the proportions of gypsum, the method of seasoning, and the like are contributory factors. Uniform chemical composition of the raw mix has been one of the most difficult problems to solve. Most plants will use from 1000 to 3000 tons of rock per day and in but few cases is this material as it lies in the quarry even approximately uniform in composition. The problem, then, is to quarry and mix this raw material in such a manner that every handful passing through the kilns will have practically the same analysis as every other handful. To accomplish this purpose there are two methods of preparation: the wet and the dry. In each process, a stone storage is the first requisite of a successful plant. This storage place may handle the stone before or after crushing; its capacity may vary from two to three days' up to several months' supply, but it should be so designed that it can be filled as desired by the chemist and drawn at such points as will give a mixture of the various kinds of stone coming from the quarry and a reasonably uniform material going to the mill. The size of the storage place and the method of handling should be varied according to the nature of the material.

Jan 1, 1925

By K. A. Slagle

Hydraulic analysis of the wellbore has become increasingly inzportant for designing cementing operations and selecting equipment, materials and techniques to complenzent modern well-c-ompletion practices. Non-Newtonian fluid technology has advanced beyond the point where former empirical methods of analysis adequately define the hydraulic system and fluid properties. In view of these factors, this paper describes a series of rheological calculations which have been found practical, through field usage, for assistance in selecting a cementing program. A relatively simple laboratory method using standard viscometric equipment is suggested for determination of the rheological properties of slurries, and clrrta are presented on some of the more common cementitrg conzposition.A. A criterion for divergence from laminar-flow characteristics has been proposed. Usefulness of the calculations is indicated by examples of cementing operations where they have been used. INTRODUCTION With the changing aspects of well-completion practices during the past few years, it has been increasingly important to have a relatively simple method of analyzing the flow conditions existing in the well during cementing operations. This is particularly true in view of the improved economics toward which most of the changes have been directed. Rheological characteristics of slurries used for cementing should be a major consideration in the trend toward smaller casing sizes, either single or multiple strings. Receiving increased attention is the practice advocated in 1948 by Howard and Clark' of attaining turbulent flow with the fluids circulated during a primary cementing operation. While there may still be a difference of opinion concerning this technique, most available information indicates that superior primary-cementing results are generally obtained when high displacement rates are employed. Fluid properties of the slurry to be used must be available, as well as calculation methods, to determine what flow rates should be attained and the probable consequences in terms of frictional pressure and horsepower utilization. It would certainly be inappropriate to attempt high displacement velocities if sufficient pressure might be developed to create lost circulation. Since cementing slurries are non-Newtonian fluids, it is not possible to define their rheological or fluid properties by the single factor of viscosity and then make calculations for the quantities just described. Because the shear stress-shear rate ratio is not constant: it becomes necessary to establish at least two parameters for adequate fluid-flow calculations. It is not the purpose of this paper to delve into the mathematical development of non-Newtonian technology, nor to discuss the arbitrary classification system under which a single fluid may resemble two or three different classes depending upon experimental conditions. Rather, the intention is to present a useful series of calculations based on a concept applicable to both Newtonian fluids and to the preponderance of non-Newtonian fluids encountered in the oil-producing industry. Development of this approach was begun some 32 years ago,' and has most recently been brought to fruition by Metzner and his co-workers at the U. of Deleware. Some non-Newtonian fluids encountered in the petroleum industry, other than cementing slurries, have also had the benefit of this method of analysis."' The two parameters required to define the fluid are usually denoted by the symbols n' and K' and, for the purposes of this discussion, are called "flow behavior index" and "consistency index", respectively. These two slurry properties permit calculation of the Reynolds' number and the "critical" velocity, or the velocity at which departure from laminar flow begins. EXPERIMENTAL DETERMINATIONS The two principal instruments used for rheological studies are the pipeline (capillary-tube) viscometer and the rotational viscometer. When conveniently possible, a capillary-tube viscometer (where the pressure drop and flow rate of the material can be measured) is the better method for rigorous determination of the flow behavior index and consistency index for non-Newtonian fluids. With pressure-drop data at various flow rates, it is then possible to prepare a logarithmic plot of shear rate as the abscissa-shear stress as the ordinate. For fluids which do not exhibit time-dependency, these data will usually produce a straight line. The flow behavior index n' represents the slope of this line, while the consistency index K' becomes the intercept of this line at unity shear rate in accordance with the mathematical derivations associated with this concept of rheology. Due to the difficulties anticipated in maintaining a uniform, pumpable cement slurry for the time interval required to obtain measurements from the pipe viscometer, the n' and K' data reported herein were obtained using a direct-indicating rotational viscometer (Fig. 2). The

By Fenton Scott, Patrick Hannon

Some occurrences of lead-zinc mineralization in Mississippian carbonates of central Nova Scotia are briefly described. The results of geophysical and geochemical prospecting are presented. Because the deposits do not give a positive response to these indirect techniques it is necessary to site exploratory drilling through the development of geological concepts.

Jan 1, 1976

By John F. Havard, Armine F. Banfield

Sooner or later, we all get involved in the economic study and valuation of a mineral deposit. To communicate clearly the necessary information, we must scrupulously use various terms with specific meaning. All these terms-such as ore, exploration, development, production, reserves, proven ore, probable ore, possible reserves, resources, as well as similar terms applying to coal-are continually on the lips of anyone who reports on the economic aspects of a mineral deposit at the exploration, development, and production stages. The meaning of these terms is even more important in feasibility studies to determine whether a deposit should be put into production. Finally, careless use of these terms in reports published for public financing may, and sometimes does, lead to prosecution of the writer for misleading information.

Jan 7, 1975

By S. A. Herres, A. R. Elsea

Temper brittleness refers to the loss in the notched-bar impact resistance encountered in most medium- or low-alloy steels when they are tempered within the temperature range of 700 to ll00°F or slowly cooled from a higher tempering temperature. Temper brittleness is important because it impairs the service properties of otherwise suitable steels over the range of hardnesses obtained at medium tempering temperatures and because it is impractical to cool pieces of large section rapidly enough from higher tempering temperatures to prevent temper brittleness. The problem of temper brittleness has always been closely associated with ordnance manufacture because armor plate and gun steels require good shock resistance and are often heat treated in heavy section. However, it is now realized that many brittle failures in structural alloy steel parts are attributable to temper brittleness, and there is little question that it contributes to the low impact resistance of alloy steels used in the hot-rolled or normalized condition which are slowly cooled from the hot-rolling or normalizing temperature. Recently Hollomonl has presented a comprehensive summary of the literature on the subject and an excellent description of the manner in which temper brittleness affects the notched-bar impact resistance and other mechanical properties of steel. Carpenter and Robertson2 have given a good analysis of the probable mechanism of temper brittleness, which is similar in many respects to the precipitation-hardening phenomenon. Fig 1 is their diagram illustrating the response to tempering of a susceptible steel. Three changes are recognized as the temperature of tempering a previously quenched steel is raised: (1) pre- cipitation occurs more rapidly and to a greater extent and the notched-bar impact value falls to a minimum; (2) coalescence of the precipitated particles begins to be effective and the impact values for both rapidly cooled and slowly cooled specimens increase; (3) the precipitate goes back into solution at higher tempering temperatures and the impact values of specimens cooled rapidly enough to retain the solution increase, while reprecipitation occurs in slowly cooled specimens and their impact values decrease again. No change must proceed to completion before the following one begins and there is overlapping in temperature ranges. Although there have been a large number of experimental investigations of temper brittleness, insufficient evidence has been accumulated to permit definite identification of the precipitate wnich causes temper brittleness nor have the specific effects on it of various alloy elements and impurities in steel been definitely established. This lack of evidence is largely a result of the lack of a suitable measure for temper brittleness. Temper brittleness is evidenced by an increase in the temperature of brittle failure of notched-bar impact specimens, but most of the data are in the form of an arbitrary susceptibility ratio of the room-temperature impact value for specimens quenched from a high tempering temper to that of similar specimens furnace cooled from the temper. It is obvious that this numerical ratio is dependent upon the type of specimen used and the specific conditions of testing rather than the characteristics of the steel. In general, manganese, chromium, and nickel alloy steels are most susceptible to temper brittleness and molybdenum has heen used to decrease

Jan 1, 1950

By Robert R. Turner

This paper discusses wet and dry primary autogenous and semi-autogenous grinding, including a description of the equipment and its mode of operation, testing and the scaling-up of test data. Lists of selected literature references are included.

Jan 1, 1982

By J. B. Shannon, J. D. Grenia

The Buick Mine is a joint venture of American Metals Climax, Inc. and Homestake Mining Company located 120 miles by road southwest of St. Louis, near the village of Boss, in the `New Missouri Lead Belt'. Since start-up in 1969, over four million tons of lead-zinc ore have been mined and milled at Buick. Situated 1100 ft below the surface at an elevation 270 ft above sea level, the flat lying sinuous orebodies are up to 250 ft wide, 85 ft high and several thousand feet long. Mineralization is galena, sphalerite and chalcopyrite in dolomite.

Jan 7, 1973

By Russell G. Haworth

Three companies, United States Potash Company, Potash Company of America, and International Minerals and Chemical Corporation, are now operating potash mines and refineries in the Carlsbad, New Mexico, area. The three mines are located approximately twenty miles east of Carlsbad. The deposits have been found ideal for mechanized mining methods. This summary has been compiled from information made available by the three operating companies.

Jan 1, 1949

By M. C. Fuerstenau, R. K. Price, R. D. Wellik, B. M. Wakawa

Median lethal concentrations of pure and commercially available ethyl xanthate, isopropyl xanthate, amyl xanthate, diethyl dithiophosphate, dibutyl dithiophosphate, and isopropyl ethylthionocarbamate for rainbow trout have been established utilizing static bioassays.

Jan 1, 1975

By C. K. McArthur

THE subject of classification is so broad that this discussion is confined to what the author believes is of prime importance in connection with proper grinding and classification. The years passed have witnessed many noteworthy changes in fine grinding and classification, which have been accompanied by a readjustment of ore-dressing flowsheets for the preparation of better ground and/or sized products at an expenditure of less power, steel and maintenance than formerly. Nowhere in the industry is more being done in the way of experimental work to lower costs than in grinding circuits, because, at best, grinding costs are high. Recent years have indicated that, on the average, finer grinding has a real application. Without careful preparation of the process feed, no operation can be highly efficient or successful. In an earlier paper, the findings of an extensive survey at representative concentrators were presented1. Also, in the year of 1935, a technical discussion was given by Dr. J. V. N. Dorr (Some Notes on Classification Trends in America) before the Chemical, Metallurgical and Mining Society of South Africa In both papers mentioned, much has been said regarding flowsheets, grinding and classification. The author is very familiar with these papers, having had considerable to do with the actual operation of the flowsheets, as well as large mills and classifiers in the work described. Some data from the second paper have been included in the following discussion. Circulating Load In this particular paper it seems advisable to deal with the classification phases of the work that to a major extent govern the success of any closed-circuit grinding unit. The question has often been asked in connection with a closed circuit: "What circulating-load ratio should be carried?" This is really an

Jan 1, 1937

By D. Watson, T. J. N. Grainger-Allan

A technique for studying the mechanism of the froth flotation process in which continuous froth removal does not take place but, instead, an equilibrium is reached between froth and pulp is described. A flotation cell, specially designed to facilitate equilibration, and froth and pulp sampling procedures are described. The main advantage of the technique is that the ability to measure the steady-state froth height allows froth-stability effects to be separated from pulp-process effects. In the flotation of hematite front quartz, linear relationships are found between airflow rate and froth height and between airflow rate and the ratio at equilibrium of mass of values in froth to mass of values in the pulp. A simple mechanistic interpretation of these results is given. It is suggested that froth-stability effects may play a more important role than hitherto allowed. In particular, the way in which concentration and size distribution of gangue particles may affect overall flotation rate is shown.

Jan 1, 1975

By Norman Gerald

THE lack of a continuous operating balance in petroleum refining, which is analyzed in this paper, is by no means a feature solely of this division of the oil industry. Serious disequilibria of a capital as well as an operating nature exist both in the producing and marketing departments, while problems in the former and to some degree the latter are complicated by political involvements. Attention has previously been directed to the unstabilizing influence of present proration formulas in stimulating unnec-essary drilling.1 While equilibrium in petroleum refining operations has been fairly well maintained in the past decade, examination of departures may prove fruitful. Economic analysis is the application of time and motion study to the functioning of management, rather than labor. Properly applied it may reveal changes in policies that would increase the utility of the properties and facilities of the industry for stockholders, employees and the public, while contributing a stabilizing influence to the general economy. The study of economic equilibrium is essentially one of measurement and interpretation, requiring adequate data and the development of a tech-nique of analysis that employs statistical and mathematical methods as a supplement to the broad descriptive phase of economics. Economic equilibrium in petroleum refining is a dual concept. It embraces both the over-all balance between total storage and total demand for major products and the internal balance between the demands and inventories of the various products. The latter is the more complex of the two for it is concerned with proportionating the supplies of the several products stemming from the joint source to the demands for the individual products which are subject to wide variations. All the products are essentially nondurable goods, and they are used both by producers and consumers but in varying proportions. Motor fuel is very largely a consumer's good, while residual fuel oil is almost entirely a producer's good, the other products falling between these extremes. The peculiar-

Jan 1, 1939

By Hewitt Wilson

CHALK is soft, pulverulent limestone formed from calcareous remains of microscopic organisms. Whiting is the powder made by the fine- grinding of limestone. Although European chalk dominated the early American market and is still shipped to the eastern and western seaboards, the domestic producer, by new technical processing, improved equipment, and proper selection and mixing of raw materials has shown that the United States can be independent of foreign sources. DISTRIBUTION European Chalk-Outcrops of Cretaceous chalk are found in the area roughly bounded by Antrim, Ireland, on the east, East Prussia on the west, Sweden and Scotland on the north, and Nice, France, on the south. Commercial chalk is mined from the chalk cliffs between Dover and Hull, England; from deposits near Mons, in the Departments of Pas de Calais and Nord in northern France; and from similar de- posits in Denmark and Belgium. United States-Some grade of limestone is found in every state of the Union, but true chalk of Cretaceous age is limited to three large areas in the central and southern states. Niobrara (Cretaceous) chalk outcrops are found as a narrow band encircling the Black Hills in South Dakota, Wyoming, and Nebraska, and in much larger exposures in southeastern South Dakota, eastern Nebraska, and western Kansas. A third chalk belt extends from west central Arkansas into Oklahoma and connects with the Austin beds, which almost cross Texas. In the southeastern states, the Selma chalk extends from western Tennessee south through northern Mississippi and turns east across central Alabama. Most of the domestic chalks are discolored with iron oxide or carbon. Some marls can be included with chalks of commercial possibilities. Some of the soft, cream-colored limestones of northern Florida, Georgia,

Jan 1, 1949

By D. M. Kehn

A method has been devloped for chromatographic analysis Of the vapor and liquid phases Of a a system containing methane to components having 20 or more carbon atoms. The method uses a windowed equilibrium cell in which volumetric phase behavior of the system can be observed accurately and from which small samples of gas or liquid can be withdrawn for analysis. Analyses are made using two chromatographs, one for the lighter and one for the heavier components in a sample. Combination of the two analyses yields a detailed analysis of the gas or liquid sample. The complexity of the condensate heavy ends is evident from the chromatograms of these fractions, and the predominance of the paraffin hydrocarborn serves as a useful marker in interpreting the chromatograms. The K-values obtained in this analytical method are presented for a high-pressure condensate system and predict closely the observed volumetric behavior of the system. INTRODUCTION Quantitative analysis of hydrocarbons from natural gas reservoirs is necessary for several reasons—to calculate the amount of sales gas produced, to calculate the amount of natural gasoline produced, to plan a liquid recovery system, or to calculate the potential economic value of a reservoir produced under one or more of several different conditions. Analysis of natural gas fluids produced to the surface consists of identifying and computing the mol fraction of each component of the mixture. Although methane is the predominant component, varying amounts of ethane, propane, butane, pentanes and heavier components are also present. Materials containing up to 30 carbon atoms occur in amounts which decrease with increasing molecular weight. However, the quantities of components in the 20 to 30 carbon atom range are usually so small that their importance is negligible, and they are undetect-able in natural gas by ordinary analytical methods. All the components up to those having 20 carbon atoms may sigsficantly affect phase behavior, however. Commonly, only the methane-through-pentane fraction is analyzed quantitatively for each component, while components heavier than Pentane are lumped and repored as "hexane- plus". Expensive, tedious techniques are required for analysis of this fraction. Consequently the detailed analyses needed for prediction of reservoir behavior are usually undertaken only when major gas fields are being developed. The need for complete analyses of condensate systems is apparent when it is recalled that most gas fields are produced by pressure depletion. As the pressure declines, some of the heavier hydrocarbons are lost as liquids which are in the reservoir. In many instances the amount of liquid in equilibrium with the gas phase at high pressure constitutes only 1 or 2 mol per cent of the total system. Flash calculations generally must predict the actual amount of liquid with an accuracy of a few per cent in order to be useful. This retrograde condensation has been understood for years, but accurate correlation methods to permit quantitative prediction of phase behavior in the retrograde region are not presently available. The increasing importance of natural gas has made accurate prediction of phase behavior and composition of produced natural gas streams an economic necessity. The work reported here was undertaken to provide a rapid, economical method for obtaining the vapor-liquid equilibrium information needed to predict accurately the composition of the fluids produced from a gas reservoir throughout its life. TO develop this method, a pressure cell equipped with windows was designed and built for observing the volumes of liquid and gas present at reservoir pressures and temperatures. Use was made of established chromatographic methods for rapid and detailed analysis of both phases. This paper describes the equipment and techniques developed for obtaining vapor-liquid equilibrium data, presents the results of analyses of a condensate system, and indicates the usefulness of these data in predicting hydrocarbon phase behavior. DESCRIPTION OF EQUIPMENT USED The equipment used in obtaining the required information on phase behavior and the complete analysis of hydrocarbon mixtures through C, will be described first, followed by a discussion of the operation of the equipment. It will be helpful, however, to consider first a brief outline of the technique used. A sample of separator gas and liquid is charged to the windowed cell (see Figs. 1 and 2) where volumetric equilibrium phase behavior at reservoir pressures and temperatures can be determined. Then samples of the coexisting phases are withdrawn. The methane-through-pentane fraction is analyzed with a chromatograph equipped with a hot-wire detector, and the pentane-plus fraction is analyzed with a second chromatograph equipped

Jan 1, 1965