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By J. D. Sullivan, Chester R. Austin, J. L. Nunes

It is characteristic of most shales and surface clays that a bloated or vesicular structure is produced by burning to a sufficiently high temperature, usually about 150° to 200°F. above the normal maturing temperature used when making common brick of the same material. Early investi-: gators recognized this phenomenon and attributed it to the release or expansion of gases in the vitrified piece. A number of theories have been advanced on the source of the gas and the manner in which it is evolved, but none has been proved conclusively. T. E. Jackson's1 early theory that bloating was due to oxygen evolved by ferric oxide in forming ferrous oxide or ferrous silicate was never substantiated by - experimental work. Orton2 thought this explanation unlikely, as all clays should bloat at the same temperature, if this were true. He found that clays bloated in the range from IIoo° to 17oo°C. Also, many clays containing iron did not bloat at all, but fused. Orton also stated that oxida- tion of different types of carbon was a source of gas during burning of clay and should be expelled before vitrification was reached. Seger3 said that he had dissolved ferric oxide in glass with no apparent evolution of gas. Matson4 came to the conclusion that ferruginous clays burned ' to vitrification in an oxidizing atmosphere did not have the iron in a ferrous form. According to Wilson,= the gases responsible for bloating might be entrapped air, water, sulphur dioxide, carbon monoxide, oxygen, and hydrocarbons. He spoke of two causes of bloating: (I) incomplete oxidation below the vitrification temperature, and (2) decomposition of compounds and evolution of gases above the vitrification temperature. Decomposition of calcium sulphate was given as the principal example of the latter. Bleininger and Montgomery0 stated that if any time after vitrification began the evolution of gaseous matter was rapid enough so that pressure was produced within the clay, bloating was certain to take place, and a vesicular structure would be formed. They recognized that initial structure, rate of heating, kiln atmosphere, and many other variables affected bloating. Work done by the Emergency Fleet Corporation7 indicated that clays suitable for bloating should be high in compounds of metallic oxides, carbon, sulphur, sodium, potassium, or other equivalent compounds, which either act as a flux or give off gas. Orton2 studied the chemical status of the carbon, iron, and sulphur in clays during various stages of burning, using a Huron shale that bloated under oxidizing or reducing conditions. He found that only a small amount of sulphur remained in the clay and that it could be detected only by dissolving the clay in hydrofluoric acid; i.e., the sulphur was in combination with the silica. orton said that this sulphur was probably in the form of iron sulphide dissolved in the glass phase. The iron sulphide was not broken down by heating, but was dissolved in the basic slag or glass,

Jan 1, 1942

By N. A. Gjostein

The formal descnption of the decay of an isolated scratch can be written in terms of an appropriate Fourier integral. With the application of certain approximations, this description leads to the second-moment analysis developed by King and Mullins. It is shown that the second-moment analysis does not adequately describe the behavior of a decaying, isolated scratch, and that it is difficult to obtain internally consistent values of the surface self-diffusion coefficient, D,,from this analysis. This inconsistency arises from contributions of higher-order moments to the decay process. Two new analytical methods, based on the Fourier integval representation of a scratch profile, have been developed for determining values of D, from the decay kinetics of isolated scratches. In the profile-matching method, a given initial profile is resolved into its Fourier components, the components are allowed to decay exponentially over an annealing time interval, At, and finally they are synthesized to form a decayed profile. The predicted profile is adjusted to fit the experimental profile by varying only the parameter, D,At; the contribution from volume diffusion is directly taken into account and the integrals involved in the Fourier analysis are evaluated by numerical integration on an electronic computer. In the kinetic method, the widths, W, of a series of predicted profiles are determined for various volume-diffusion contributions, and the results are plotted in the form W vs DSAt. For a fixed ratio of surface to volume diffusivities, R, these plots are linear; the slope of the lines increases as R decreases. A simi-lar analysis can be performed on the depths of the predicted profiles. In this case, plots of (l/df3 vs D,At are found to be nonlinear. The proper value of Ds is found by superimposing the data for the experimental widths and depths on Plots of this kind and adjusting Ds until a fit is obtained with the line having the appropriate value oj R. An analysis of the slopes of these plots for R —= (surface diffusion only) reveals that they do not give the correct value, 2276, for width tf second-moment standard profile. This finding allows one to modify the second-moment analysis in such a way as to obtain internally consistent values of Ds. ThERE are several processes, involving a flow of matter along a surface, due to gradients in curvature of the surface, that may be used to determine the surface self-diffusion coefficient, Ds. These processes are commonly known as 1) thermal grooving, 2) single and 3) multiple scratch decay, 4) blunting of field-emitter tips, and 5) sintering. In this series of papers, the first three of these processes are examined in detail in an attempt to subject the phenomenological theories governing these processes to a critical test and, furthermore, to make a critical comparison of the values of D, obtained from these techniques. Although the thermal grooving technique has been established'' as a reliable method for determining D, , this has not been the case for the process of scratch flattening. Mullins and coworkers374 have proposed phenomenological laws governing the growth of the width and the decay of the amplitude of an isolated scratch, but only in one study5 has the width-growth law been supported by experimental evidence. In paper I of this series detailed experimental evidence is presented that points up the deficiencies of the second-moment analysis; the origins of these deficiencies are also discussed. Following this development, some new analytical procedures, based on representing the scratch profile by Fourier integrals, are presented as a means of obtaining reliable values of D, from the kinetics of the scratch-flattening process. Further applications of the Fourier integral approach are reported in papers 11' and 111,~ where the method has been useful in interpreting the anisotropy of flattening rates of isolated scratches (paper 11) and in describing the multiple scratch decay process (paper 111). THEORY OF SCRATCH DECAY Following ~ullins" approach we consider an arbitrarily shaped scratch profile, Fig. 6, at some time, t. The profile is designated by a function z(x,t) which can be expressed in terms of a Fourier integral as follows:

Jan 1, 1967

By Joseph Chalmers

PROBLEMS dealing with the movement or ,migration of fluids through porous beds have been the subject of much research. The subject is not peculiar to the production of oil and gas, as many investigators have studied the nature of this movement and its relationship to the problems of other industries. Darcy1 conducted a series of experiments relating to the percolation of water through filter beds. King2 carried on an extensive series of laboratory experiments with the object of formulating some conception of the rate of movement of water through soils and sand strata in the drainage of surface water into underground channels and subsequent recovery of this water through wells drilled into the source beds for irrigation purposes. Slichter3 undertook a study. of the same problem from a mathematical standpoint, and more recently Furnas4 has investigated the flow of gases through beds of broken solids with particular reference to blast-furnace operation. With specific reference to gas production, Muskat and Botset5 of the Gulf Research Laboratory undertook an experimental study to establish quantitatively the characteristics of and laws governing the flow of gases through consolidated and unconsolidated porous materials of fine texture with a view of predicting the performance of gas in an underground reservoir. There seems to be a general agreement that many of the relationships between the numerous factors influencing the flow of fluids through porous materials are far too complicated to be attacked by analytical methods based upon a knowledge of hydrodynamics. For gases, the laws of

Jan 1, 1932

By George Norman

A NUMBER of methods have been developed for the determination of the dust concentration in air, some of which have been reported as very efficient and for research may be more satisfactory than the method about to be described. In practical mine use, however, the accurate research equipment is unwieldy and requires a high degree of technical skill to manipulate it. Also, it gives less general practical information to the operator in the same length of time than the method described here. Moreover, it is doubtful whether at the present stage of affairs the results obtained from the precise methods have any more practical significance than those obtained with simpler and more portable appara-tus, which can rapidly give a sufficiently reliable indication of the rela-tive dust hazard.

Jan 1, 1937

By ELTCENE A. WHITE

WE are all interested in our ou7n lines of endeavor and consider ourselves the center of the universe. The farmer thinks he is the most important man because he feeds us. The doctor knows he is the real center because he keeps us well. The lawyer says that he is indispensable because he keeps the peace. The banker furnishes us a place to keep our money and tells us how to make proper use of it. The miner sags that without metals there would be no civilization. I think that my branch has sufficient interest and exhilaration. of accomplishment to fully occupy any man's mind and attention. Mining and metallurgy are as old as the human race. It did not have much, if any, importance in the stone age as there are not found remains of iron and copper, but in the bronze age, which was co-existent with the stone age, it came to the front. Iron and copper were the most important metals. Copper, as bronze, was known in ancient Egypt, I\~:IS important in Rome and other parts of Europe and in Asia; in South America among the Aztecs and farther North were the Mound Builders and the early inhabitants of Lake Superior. At a very early date the Egyptians conquered the Sinai peninsula for the sake of the copper produced there. The history of copper metallurgy can be compared to that of a flower. The seed is sown in darkness and in the Dark Ages the crude metallurgy of copper began. As the shoot comes up from the seed it may be compared to the age of alchemy; the branches of the plant can be compared to the Middle Ages; the flowering shoots to the 17th century, the budding to the 19th and the blossom to our own time from 1870 on.

Jan 1, 1930

By A. H. Larson, R. J. McClincy

Laboratory-scale decopperizing experiments with multiple sulfur addifions were conducted at 330°C on ternary Pb-Cu alloys containing, as the third elenlent, Sn, Ag, As, Sb, Bi, Zn, and Au, common impurities in lead blast-furnace bullion. For silver and tin, an increased rate and extent of 'cofifier removal was obsert3ed. The elements As, Sb, Zn, Au, and Bi had no effect or less effect as compared to sulfur additions with no i)npurily additions. THE production of primary lead in the blast furnace yields an impure lead frequently containing such impurities as copper. antimony. arsenic. tin, gold, silver iron, oxygen. and sulfur. By cooling this lead to a temperature near its melting point. most of the iron, sulfur, and oxygen and part of the other impurities are removed in the form of a dross. With incipient solidification of the lead, the copper concentration wil have been reduced to 0.02 to 0.05 pct. depending upon the concentration of the other impurities. according to Davey.' Since copper interferes with the treatment of silver after the desilverizing process, it is desirable to decrease the copper content of the lead still fur-ther before the lead is desilvered. The decopperizing of the lead is accomplished by stirring a small quantity. approximately 0.1 pct. of elemental sulfur into the lead at a temperature near its melting point, 330" to 360°C. The copper is removed as a copper sulfide which constitutes a small fraction of a voluminous dross consisting mostly of lead sulfide and entrained metallic lead. The residual copper concentration following the decopperizing operation is frequently as low as 0.001 to 0.005 pct. Thi fact has aroused considerable interest because the equilibrium copper concentration of lead in contact with solid PbS and solid Cu2S is at least an order of magnitude greater, 0.05 pct Cu at 330C. 1, 2 Most investigators have suggested that various impurities in the lead bullion are responsible for the very low copper concentrations frequently encountered in practice. There is little agreement, however? as to which of the impurities are helpful and which are not.3"11 Also. few investigators have sought to explain the mechanisms responsible for the removal of copper to very low concentrations. Willis and Blanks9 have proposed that a nonstoichiometric copper-deficient cuprous sulfide forms in place of the supposed Cu2S. Being copper-deficient, this sulfide phase would possess a low copper activity, and the diffusion of copper dissolved in the liquid lead into this phase would be greatly facilitated. Pin and wagner2 have investigated the removal of copper from liquid lead by studying the effect of impurity-doped lead sulfide on the decopperizing of pure Pb-Cu alloys. Samples of the doped PbS were held in contact with copper-saturated lead for 1 week at 33'7°C. They reported a beneficial effect on decopperizing with bismuth and antimony and no effect with tin or silver. which is directly opposite to the results observed in practice and those reported by Davey 3 and this studv. The purpose of this paper is to describe the effects of certain additive elements on the extent to which copper can be removed fro111 liquid lead by successive additions of sulfur. The impurity elements were added individually to prepared Pb-Cu alloys. The resulting ternary alloys as well as a binary Pb-Cu alloy were then decopperized with repeated additions of sulfur. EXPERIMENTAL Materials. Granulated test lead with a purity of 99.999 pct and the additive elements Cu. Ag. Sb. Bi. Zn. Sn. and Au with purities of 99.99 pct were American Smelting and Refining Co. research-grade materials. The major impurities in the lead were 1 ppm each of iron and copper. all others being less than 1 ppm. The arsenic used was a technical-grade arsenic of 98+ pct purity. Reagent-grade flowers of sulfur were melted under argon to provide small pieces free of fines. Apparatus. The decopperizing experiments were carried out in a 25-mm-OD by 375-mm-long Pyrex tube sealed at one end. The tube was mounted vertically in a resistance-heated. hinge-type tube furnace controlled to within ±lcC. Temperature measurement was accomplished by means of a standardized chromel-alumel thermocouple sealed into the base of a silica. paddle-type stirring rod. All decopperizing experiments were carried out under an argon atmosphere. Procedure. A Pb-Cu starting alloy containing 0.05 pet Cu was prepared under carbon and poured into cold tap water to produce shot. The ternary alloys were prepared by melting together 100 g of the starting alloy and a sufficient amount of the impurity element to yield the desired concentration. The resulting alloy was then homogenized in a Pyrex tube at 450C with continuous stirring. The furnace temperature was then lowered to the operating temperature of 330°C. When thermal equilibrium had been obtained at the operating temperature, individual additions of 0.2 pct (0.2 g) of solid sulfur were added to the melt and stirred in. Stirring was continued for a period of 3 min. discontinued for 5 min. and resumed for the remaining 2 min of a 10-min cycle. This cycle was repeated for as many sulfur additions as desired. When the decopperizing experiment had been completed the lead bullion was quenched and samples of the bullion and dross phases were taken for analysis. Results. The results obtained in the decopperizing

Jan 1, 1970

By AIME AIME

THE Engineering Education Committee of the Institute convened at the Engineering Societies Building on Feb. 18, .1929, with. E. A. Holbrook, dean of the Schools of Mines and Engineering, University of Pittsburgh, in the chair. STATISTICAL' STUDY OF STUDENTS IN MINING The first paper, a statistical study of the students enrolled in courses leading to a mining degree in 40 institutions, was presented by H. D. Keiser,, assistant editor of the Engineering and Mining Journal; who gave a brief outline of an article he was about to publish in ?that journal?. The complete article appears in the issue for March 30; 1929: To avoid repetition the results are summarized as follows: A request was sent to 42 institutions which give courses in mining' for the number of students enrolled as freshmen; sophomores; juniors, seniors and special students in mining for the years 1925-26, 1926-27, 1927-28, 1928-29. Two of these colleges replied that there were no students in mining. Students' enrolled in courses in metallurgy, geology and engineering, other than mining, were excluded from the statistics:. The statistics received were arranged in, four groups, according to the completeness of the information. One complete group of 25 institutions 'shows as follows:

Jan 1, 1929

By P. R. Sperry, M. L. Holzworth, P. A. Beck

The basic work of Z. Jeffries 1,2,3 has long ago established the main features of grain growth in the presence of a dispersed second phase. Working with sintered specimens of initially fine grained tungsten, to which various amounts of thoria had been added, Jeffries found that grain growth was inhibited, that is, practically prevented, up to a certain annealing temperature. When this temperature, which increased with the thoria content, was exceeded, extremely large grains developed abruptly from the fine grained matrix. such a a temperature" was later found by Gross-mann~3,14 in certain types of steel, while ~~i~ showed15 that in other steels grain growth was gradual, without inhibition and abrupt coarsening. Later work demonstrated the connection between coarsening and aluminum additions. The viewpoint that the direct cause of inhibition and coarsening in aluminum killed steels is a fine dispersion of aluminum oxide21 appears to be held quite generally, although some doubts have been voiced even very recently, 20 In steels with Ti additions the titanium carbide phase is considered responsible for the inhibition effects found.20 The coarsening temperature increases with the titanium content. That coarsening may occur, as a result of, certain heat treatments, even in low carboil rimmed sheet steel, was shown by Samuels. He also detected coarsening in a steel ingot of similar composition, after giving it the same heat treatment as that used by him for the sheet material. In this instance the identity of the inhibiting phase has not been determined. However, Tangerding found23 that even the few small carbide particles, which occur in carbonyl iron, have a very marked inhibitive effect. As a result of an oxidizing anneal at 850°C, large grains begin to form at the surface of the carbonyl iron specimen, and gradually grow inward as the subsurface oxidation of the carbide particles progresses and eliminates the obstruction. The carbide particles Can be removed also by annealing in hydrogen, with similar results. But if the oxidizing anneal of 10 hr at 850°C in air is followed between in hydrogen for 75 hr at the Same temperature, grain growth is more hibition usually the whole specimen is transformed into a single crystal (approx. 1.5 cm X 5 cm). The reversed procedure, that is, hydrogen annealing followed by oxidizing annealing leads to smaller grains. Tangerding arrived at the logical conclusion that there must have been in his specimens some additional obstruction to grain growth hibition from a minor impurity, other than carbon. It seems likely that this obstruction was caused by an oxide formed during the oxidizing anneal and gradually reduced rtain the subsequent hydrogen-annealing. Other instances of grain growth inhibition of varying severity, associated with a dispersed second phase, have been described by several authors. Notable examples: lead with 0.06 pet Cu or Ni,24 cartridge brass with 0.12 pct Cr,25 or with up to 0.15

Jan 1, 1949

By W. J. Taylor

Every one having practical experience in making heating-gas knows how much room there is for improvement,, in order to avoid not only the production of poor gas, when good gas is most wanted, but also the waste due to burning gas on top of the fuel-bed, and the loss of both time and fuel in cleaning.* The producer which I have recently designed, and with which I am now experimenting with every prospect of success, at the oreroasting kilns at Chester furnace, is intended to remove these difficulties as far as possible, and at the same time to be continuous in operation. I have not had it at work long enough to get beyond the stage of experiment; hence, I will only at this time explain it in a general way, and illustrate it with a drawing, promising a more elaborate paper if it becomes the practical success I anticipate. The features of the producer are : 1st. The round dome-shaped revolving bottom; and 2d. Metallic water-cooled walls in place of the usual brick lining. As shown in the drawing, the bottom has a sleeve, which fits over the air-admission pipe, coming up through the center of the

Jan 1, 1887

By C. E. Silverblatt, D. A. Dahlstrom

Previous bench-scale studies demonstrated that a substantial moisture reduction can be obtained by the application of steam to coal filter-cakes, particularly to those containing a limited amount of minus 200-mesh material. Consequently, U.S. Steel's Applied Research Laboratory conducted a study to determine the feasibility of steam filtration of 1/4 in. by 0 coal on a continuous pilot-scale installation in which an Eimco extractor is used. The test results showed that the moisture content of this coal could be reduced to 5.5% at a steam loading of about 175 lb of steam per ton of dry cake. In terms of steam consumption, this loading is calculated to be 1-1/2 lb of steam per lb of water removed. In some tests, only 1 lb of steam per lb of water removed was required. These levels of steam consumption are significantly less than the actual heat requirements of conventional thermal dryers. The satisfactory moisture reductions were obtained at filtration rates of 125 to 186 lb of dry solids per sq ft per hour. However, the proper design of commercial filters should improve the potential rates that can be attained. These results indicate that steam filtration has considerable economic potential for drying 1/4 in. by 0 coals and also has additional advantages over the conventional thermal drying of coal. The results of the previous bench-scale studies and those published by Burton' demonstrated that a substantial moisture-content reduction can be effected by the application of slightly superheated steam to coal filter-cakes, particularly to those containing a limited amount of minus 200-mesh material. Consequently, US Steel's Applied Research Laboratory conducted a study to determine the feasibility of steam filtration of 1/4 in. by 0 coal on a continuous basis. In the continuous process, the dewatering operation on the filter is conducted in stages. In the first, the bulk of the water in the feed slurry is removed by conventional mechanical dewatering on a portion of the filter before the steam is applied. In the second stage, steam is applied to the cake. The steam condenses and releases its latent heat, thereby reducing the viscosity of the remaining cake water; this reduced viscosity then facilitates further drainage and produces a cake of lower moisture content. Because of the availability of feed coal on a continuous basis and since steam was readily available from a low-pressure boiler, the Applied Research Laboratory selected for the test site a coal-preparation plant that cleans Pittsburgh Seam coal. A slurry of table and flotation coal in percentages as they occur normally was used as feed stock. Typical analyses of this slurry are shown in Table I. DESCRIPTION OF FILTER AND EXPERIMENTAL PROCEDURES An Eimco Extractor was selected for the evaluation of steam filtration in a continuous process. This unit was chosen because of its availability and its design features that permit relatively simple hood construction, instrumentation, and operation. A photograph of the Extractor is shown in Fig. 1. In the filter a cloth medium is used that travels horizontally and continuously with a grooved, rubber drainage belt. The total effective filter area was 12.5 sq ft. As the feed slurry flows by gravity from the feed box onto the medium,

Jan 1, 1964

By M. A. Scheil, S. L. Hoyt

About three years ago eight standard steels were prepared for the cooperative investigation of methods for oxygen analysis, sponsored by the Iron and Steel Division of the American Institute of Mining and Metallurgical Engineers and by the National Bureau of Standards. A preliminary report of the results was made at the annual meeting of the A.I.M.E. in February, 1936. † This report showed the reliability of vacuum-fusion methods and further brought out certain advantages of the fractional vacuum-fusion method. The results obtained by the authors with the latter method will be discussed here, with some comments on the procedure for those who are interested in determinations of gases in steel. Some additional comments are offered on the use of the polarizing microscope for identifying the inclusions in the steel to check and amplify the findings of the fractional vacuum-fusion analysis. For details of the fractional method, see the paper by L. Reeve1. Degassing the Crucible One of the sources of error in vacuum-fusion methods has been the blank gases evolved from the graphite crucible after preliminary out-gassing. We have used 1750" C. as the outgassing temperature. This gives a base pressure at that temperature of less than 0.030 mm. after one hour and of 0.004 mm. on dropping the temperature to 1575" C. At lower extraction temperatures the base pressure is 0.001 mm. at 1050" C., 0.002 mm. at 1170" and 0.003 mm. at 1320' C. Because of the size of our induction coil we are limited to this temperature, although it 'would be advantageous to use 1950" to 2000" C. Hamilton2, after outgassing at 1850" C. for 100 min., was able to reach a base pressure of 0.001 mm. for a temperature of 1700' to 1725" C. This would give a blank corresponding to less than 0.00015 per cent 02 and 0.00005 per cent H2. Chipman and Marshall outgas at 2000" C. for one hour by using a special construction

Jan 1, 1937

John Malcolm Fraser became Prime Minister in December 1975 when Australian voters gave him the biggest landslide victory in the history of the Federation. From the previous administration, Mr. Fraser has inherited an atrocious economic mess: a staggering budget deficit, an unrealistically overvalued currency, a 14% annual rate of inflation, mounting unemployment, and a demoralized business community. He has already tackled some of these problems with some measure of success; but he has been in power for barely a year, and it's too soon to see a turn-around.

Jan 1, 1977

By F. L. Bosqui

The history of the development of gold metallurgy in South Africa is divisible into two periods: That preceding the introduction of the cyanide process on a commercial scale in 1890; and the 24 years intervening between that important event and the present time. The period between the discovery of the banket reefs of the Witwaters-rand and the year 1890 was one of phenomenally rapid progress in mining development, but of no special interest to the metallurgist, There were no strikingly original or distinctly local advances in the treatment of gold ores. Californian practice in stamp milling and amalgamation prevailed, in mills ranging in equipment between 5 and 50 stamps, operating within a wide range of efficiency, and under the trying conditions usually encountered in a new and isolated field. The somewhat incomplete records of gold output of that period show that in December, 1887, there were 20 producing companies in the Witwatersrand district, of which 10 had mills, the largest being of 20 stamps. The only official record of returns for May, 1887, was that of the Wemmer mine, whose modest achievement with a 5-stamp mill was 100 tons crushed, producing 887 oz. 3 dwt. of gold. This is interesting in view of the present-day output of this field, which in 1913 reached 8,430,998 oz. The rapid increase of production during this first period (May, 1887, to January 1891) is shown by the following summary for the year 1890:1 Total tone crushed.................................. 702,828 Number of stamps in operation....................... 1,046 Average number of tons crushed per stamp per day..... 2.36 Yield of gold, ounces................................ 494,817 Yield per ton, pennyweights.......................... 13.36 The stamp duty ranged between 11/2 and 4 tons per day, according to weight of stamp, fineness of screen, and operating skill available. The prevailing weight of stamp was about 900 lb., and the screen, 900 meshes to the square inch.

Jan 1, 1916

By R. G. Jones, W. L. Kinney, R. E. Schilson, R. S. Wilson, G. A. Clark, H. Suralo

This paper discusses the results of the Fry conventional or cocurrent in situ combustion test, which was conduct-ed in a 3.3-acre inverted five-spot. The depth of the formation was between 880 and 936 ft; the oil had a specific gravity of 28.6° APl and a viscosity of about 40 cp at the reservoir temperature of 65°F. Preceding the combustion test, air injection tests were conducted which, in conjunction with geological studies, were used to evaluate the characteristics of the reservoir. Combustion was initiated on Oct. 13, 1961, with ignition being accomplished by a 40 kw electrical heater. The test phase of the project ended on Oct. 1, 1963. During the test, the average air injection rate was 1,520.-000 scf/D. Throughout the test, production of all fluids— gas, oil, and water—was monitored. Cumulative oil production credited to the project was 100,586 bbl. The cumulative air-oil ratio was 11,500 scf/bbl oil, and the oxygen uti1ization efficiency was 87 per cent. INTRODUCTION The Marathon Oil Co. conducted a successful in situ combustion test, beginning Aug. 22, 1961, at the Fry unit, Crawford County, 111. The purpose of the project was to test the feasibility of cocurrent in situ combustion as a means of oil recovery in the Fry type reservoir. Interest in in situ combulstion as an oil recovery tool has been stimulated mostly by the existence of large reserves of heavy viscous crudes with low expected recovery, usually less than 10 per cent. These are the so-called unrecoverable reserves, and most combustion tests to date have been conducted in this type of reservoir.1-4 In contrast, the Fry combustion test was conducted in a reservoir with a relatively high gravity oil having a relatively low viscosity. This paper discusses the performance of the test. The geology of the reservoir and the field operations are discussed in separate papers.5 TEST SITE The Fry combustion test was carried out in a 3.3-acre inverted five-spot portion of a lenticular body of Robinson sandstone. Net sand was 50 ft thick, porosity averaged 19.7 per cent, oil saturation was 68 per cent of pore volume, and water saturation was 20 per cent of pore volume. The oil in place was estimated at 1,040 bbl/acre-foot, or 171,600 bbl within the 3.3-acre pattern. The water in place was 326 bbl/acre-foot, or 53,800 bbl. The oil has a specific gravity of 28.7° API and a viscosity of 40 cp at the reservoir temperature of 65°F. AIR INJECTION PERFORMANCE Air injection took place in two phases, the phases separated by ignition of the reservoir. In the pre-ignition phase, air injection tests were conducted in the summers of 1960 and 1961. These indicated that the Fry reservoir was confined, and a high return rate of injected air could be expected. This proved to be an outstanding characteristic of the project, as cumulative gas production was 95.3 per cent of the air injected. The difference between the cumulative air injected and the total gas produced can be largely accounted for by the quantity of air stored in the reservoir. An estimated 16 X 10 cf of air remained in the burned-out portion of the reservoir and an indeterminate amount of gas was stored in the unburned but pressurized reservoir. Hence, a complete material balance of gases would account for nearly 100 per cent of the air injected. At times during the test, the daily gas production rate was 98 per cent of the daily air injection rate. Fig. 1 presents the air injection history of the Fry com-

Jan 1, 1966

By O. F. Walker, W. C. Hahn, V. A. Johnson, J. D. Wood

The diffusion coefficients of zinc in single-crystal zinc and carbon in single-crystal and poly crystalline nickel were measured by means of radioactive tracer techniques both with and without the application of ultrasonic vibrations under conditions such that the temperature of the sample was closely controlled. The results of this investigation indicate no enhancement of diffusion in any of the samples. It is suggested that previously reported enhancement may have been due either solely to temperature increases caused by ultrasonic vibrations or in combination with changes in the boundary conditions. A number of observations have been reported in the literature in which it has been implied or inferred that the application of ultrasonics enhances diffusion (see, for example, Refs. 1-5). The present study was undertaken in an attempt to observe this effect under carefully controlled conditions, particularly with regard to measurement and control of the temperature of the sample. Two different types of systems were studied; these were the self-diffusion of zinc and the diffusion of carbon in nickel. EXPERIMENTAL For diffusion with ultrasonic energy applied, the samples were included as part of a resonant ultrasonic system operating at 58.5 kcps. The ultrasonic generators used were rated at 100 and 250 w and could be tuned over a frequency from 10 to 100 kc. A PZT (lead titanate/lead zirconate) ceramic transducer provided the driving vibration. This system requires no metallurgical joining of the specimen to the acoustical transmission line since the ultrasonic driver and the follow-up section clamp the specimen in position by means of a constant pressure of 50 lb developed by an air cylinder. The ultrasonic driver and follow-up section, both made of titanium, were 4 in. in length from clamping point to the end in contact with the specimen. Using the relationship given by Mason,6 A = V/f, the resonant wavelength, A, in titanium is calculated to be 3.3 in. at a frequency, f, of 58.5 kc, taking the velocity of sound in titanium, V, as 1.95 X 105 in. per sec. The 4-in. driver and follow-up section, therefore, are each 4.0/3.3 =1.21 times the resonant wavelength. Clamping pressure must be applied at stress nodes of the transmission line in order to preserve resonance. Therefore, a specimen length of 0.58 times the wavelength in the specimen was required to place the clamping pressure application points at stress nodes exactly three wavelengths apart. A stress antinode was contained in the center 3 in. of the specimen. A small PZT ceramic disc attached to the follow-up section provided an output voltage proportional to the intensity of the standing wave. This output voltage was monitored on an oscilloscope and the ultrasonic system was tuned to resonance by varying the frequency until the output signal was a maximum amplitude. The amplitude of the output signal was maintained constant throughout the diffusion anneal. A split cylindrical stainless-steel chamber, which was purged with argon prior to and during the runs, was placed around the specimen. The chamber in turn was surrounded by a movable furnace whose temperature could be controlled to 7C. Heat exchangers were used to cool the driver, follow-up section, and ultrasonic transducer. Great care was taken to obtain the true specimen temperature in all cases. Several different methods were tried; the most successful was that in which the thermocouple was held in contact with the midlength of the specimen by means of an asbestos insulating pad and wire straps. In the case of zinc, single-crystal specimens of 99.999 pct purity were used. The samples were 0.25 by 0.25 in. square and of the proper length for resonance, that is 1.1 in. long with the c axis parallel to the long dimension of the specimen for the case of diffusion perpendicular to the c axis and ultrasonic motion parallel to the c axis, and 1.9 in. long with the c axis perpendicular to the long dimension of the specimen for the case of diffusion parallel to the c axis and ultrasonic motion perpendicular to the c axis. In each case, one of the rectangular faces was electroplated with a thin film of zinc containing Zn The constant pressure used to clamp the specimen in place in the ultrasonic system caused some deformation in some of the samples. For these samples the deformation was concentrated in either end of the specimen; thus, for all samples (both zinc and nickel) the center in. was cut from the specimen after the diffusion anneal to be used for sectioning and counting. The nickel single-crystal samples, of 99.999 pct purity, were used in the form of rods 0.25 by 0.187 by 2.07 in. long with the (100) direction parallel to the rod axis. The polycrystalline nickel samples of 99.97 pct purity had an average grain diameter of 0.007 in. and were used in the form of rods 0.25 by 0.125 by 1.87 in. long. The direction of ultrasonic motion was parallel to (100) direction (bar axis) for the single-cqstal samples and parallel to the bar axis for the polycrystalline specimens. A thin film of c14 suspended in methanol was applied to the diffusing face of the specimen. Two specimens were butted together lengthwise for each diffusion anneal to minimize oxidation. After diffusion, a precision lapping device similar to the one described by Goldstein7 and a radiation detector were used to obtain a plot of specific activity vs penetration distance for each specimen. (A scintil-

Jan 1, 1969

By B. W. Frazier

IN the numbers of the Engineering and Mining Journal of June 27th and July 11th, 1874, there appeared some very complete statistics of the working of some anthracite blast-furnaces belonging to a large establishment in this country, followed by calculations of the heat requirements of the furnaces, similar to those which have been made for European furnaces by Mr. I. Lowthian Bell, Prof. Gruner, Prof. Akerman and others. To the author of these valuable papers, Mr. John A. Church, of New York, the thanks of American iron metallurgists are due for this attempt (the first, to my knowledge at least), to attack systematically and scientifically the problem of economy of fuel in our anthracite blast-furnaces, by applying the formulas obtained from European practice and from the experiments of European metallurgists, to the determination of the amounts and the modes of distribution of the heat production and absorption in our furnaces. In order to facilitate a comparison of the results thus obtained for the anthracite furnaces in question with those obtained for the best types of European coke furnaces, I have reduced to the same standard of heat units (the product of the ton and the degree Centigrade), and placed side by side, the calculations of the heat requirements of one of the furnaces of the Clarence works, as given by Mr. Bell, of a furnace at Pouzin, on the banks of the Rhone, given by Prof. Gruner, and of the anthracite furnaces for 1869-73, as given -by Mr. Church. Table I shows the different conditions of working of the three furnaces, of which Table II gives the respective heat requirements. I have made this latter table in such a manner as to give for each furnace its heat requirements, both according to the views of Mr. Bell and those of Prof. Gruner. Mr. Bell assumes that all the carbonic acid produced by the decomposition of the carbonate of lime of the charge, is reduced to carbonic oxide by contact with solid carbon ; also, that the carbon of the pig iron is a portion of that deposited in the ore in the upper part of the furnace, by the dissociation of carbonic oxide. Prof. Gruner, on the other hand, assumes that all the carbonic acid of the carbonates of the charge escapes unreduced, and that the carbon deposited in the upper part of the furnace, by the dissocia¬tion of carbonic oxide, is again converted into carbonic oxide or

Jan 1, 1875

By J. F. Martin, L. M. Melnick, R. Rapp, R. C. Takacs

Recent studies on the determination of hydrogen in steel have shown that the hot-extraction method for removing hydrogen from a solid sample is preferable to its removal from a molten sample by vacuum fusion or by fusion in vacuum with tin. A number of techniques are available, however, for determining the hydrogen so extracted. They include: thermal conductivity, gas chromatography, pressure measurement before and after catalytic oxidation of the hydrogen to water and removal of the water, and pressure measurement before and after diffusion of the hydrogen through a palladium membrane. These techniques have been evaluated on the basis of initial cost, maintenance, speed and accuracy of analysis, and applicable concentration range. The results of this study showed that the palladium-membrane technique is best suited for routine use. FOR some time investigators have been concerned with the origin, form, and effect of hydrogen in steel. In such stdies', the analysis for hydrogen constitutes one of the most important phases. It is quite apparent that the results for hydrogen concentrations in a given steel are dependent on the method of obtaining the sample, storage of the sample until analysis, preparation of the sample, and analysis of the sample, including all the facets inherent in the calibration and operation of an apparatus for gas analysis. There are a number of means available for determining hydrogen. This is a critical study of some of the more common techniques in use today. In most conventional melting and casting methods, hydrogen concentrations of 4 to 6 parts per million (ppm) in steel are quite common. Because of the undesirable effects of hydrogen on steel there has been increased use of techniques such as vacuum melting,' vacuum casting, and ladle-to-ladle stream degassing, which lower the hydrogen content to levels on the order of 1 to 2 ppm. Therefore, the method used for determining hydrogen in steel must be sensitive and precise. In any analytical procedure for gases in metals there are two distinct operations—the extraction of the gas from the metal and the analysis of the extracted gas. To extract the gas from the steel, three methods have been employed: 1) fusion of the sample with graphite at high temperature; 2) fusion with a flux, such as tin, at a lower temperature; and 3) extraction of the hydrogen from the solid sample at a temperature below the melting point of the steel. Fusion with graphite is the least-acceptable method. The blank in this method is higher and more variable than in either of the other two methods. The hydrogen fraction of the total gas composition usually is between 10 and 50 pct; thus, a larger analytical error is possible. The vacuum-tin fusion4 extraction of hydrogen is probably the most rapid method in use today; the extraction time is usually about 10 min. However, with this system a bake-out of the freshly charged tin for 2 hr is necessary and a change of crucible and a charge of fresh tin are required after each day of operation whether one or thirty samples have been analyzed. In addition, frequent checks of blank rates are required since CO and Na are continually being given up by the steel samples dissolved in the tin bath. The composition of the gas in this method lends itself readily to analysis; although the hydroge concentration may fall to as low as 50 pct, more often it is above 90 pct, thus allowing a more precise analysis (because of less interference from other gases). In 1940 ewell' published the hot-extraction method for extracting hydrogen from the solid sample, comparing analysis for hydrogen extracted at 600°C with similar analysis for the gas extracted at 1700°C by fusion with graphite. Good agreement for hydrogen was obtained between these two methods, provided sufficient time was allowed for extraction at the lower temperature. carsone obtained good results in his comparison of this hot-extraction method with vacuum-tin fusion. Subsequent work by Geller and sun7 and Hill and ohnson' has shown that steel samples should be heated to at least 800°C to effect the release not only of the diffusible hydrogen but also of the "residual" hydrogen that may be present as methane. Since the rate of evolution of hydrogene9l0 depends on such factors as sample size and composition, thermal history, and extent of cold work, a fixed extraction time is not possible. Extraction times of 30 min are normal, but 2 hr are not unusual. Induction or resistance heating may be used in the hot-extraction method. With resistance heating the

Jan 1, 1964

By J. L. Bruce

' For a number of years, from an economic standpoint, the ventilation of the Colorado mine of the Davis-Daly Copper Co. has been a difficult problem. The development through the main hoisting shaft was pursued for a number of years and to a depth of about 2500 ft.(762 m.)before large bodies of good commercial ore were opened. This lack of early success in exploration restricted expenditures for ventilation, with the result that the present orebodies were developed at a depth of 2500 ft., and in country rock of relatively high temperature, without adequate means of supplying the development faces and the stopes with cool or fresh air of low humidity and suitable velocity. During the progress of development, two or three connections were made at higher levels with the workings of adjoining operations, but these were of a makeshift and unsatisfactory character and afforded no means for carrying downcast air from the surface, in anything approaching a direct course, to the working faces. During the latter part of 1917, arrangements were made with the Anaconda Copper Mining Co., whereby, during the year 1918 and the early part of the year 1919, a crosscut was driven eastwards on the 2500-ft. level of the Colorado shaft and connection was made by means of an up-raise of approximately 200 ft. to a crosscut driven westwards from the 2800-ft. level of the Belmont mine, this crosscut at the top of the raise being driven at Davis-Daly expense by the Anaconda Copper Mining Co. This connection, in conjunction with a No. 11 Sirocco fan installed near the Colorado shaft, provided the Colorado mine with a maximum of approximately 30,000 cu. ft. per min. of relatively fresh air, most of which came in a fairly direct route from the downcast Belmont shaft through the No. 11 fan to the 2500-ft. level stopes. After passing through these stopes and the stopes of overlying levels, it passed through the main crosscuts on higher levels back to the Colorado shaft, which provided the upcast for this current of air. The improvement noted on the completion of this work was marked, and, for a time, fairly satisfactory. Further extension of the mine workings, however, and

Jan 1, 1922

By J. L. Bruce

For a number of years, from an economic standpoint, the ventilation of the Colorado mine of the Davis-Daly Copper Co. has been a difficult problem. The development through the main hoisting shaft was pursued for a number of years and to a depth of about 2500 ft.( 762 m.)before large bodies of good commercial ore were opened up. This lack of early success in exploration restricted expenditures for ventilation, with the result that the present orebodies were opened up at a depth of 2500 ft., and in country rock f relatively high temperature, without adequate means f supplying the development faces and the stopes with cool or fresh air of low humidity and suitable velocity. During the progress of development, two or three connections were made at higher levels with the workings of adjoining operations, but these were of a makeshift and unsatisfactory character and afforded no means for carrying downcast air from the surface, in anything approaching a direct course, to the working faces. During the latter part of 1917, arrangements were made with. the Anaconda Copper Mining Co., whereby, during the year 1918 and the early part f the year 1919, a crosscut was driven eastwards on the 2500-ft. level of the Colorado shaft and connection was made by means f an up-raise of approximately 200 ft. to a crosscut driven westwards from the 2800-ft. level of the Belmont mine, this crosscut at the top of the raise being driven at Davis-Daly expense by the Anaconda Copper Mining Co. This connection, in conjunction with a No. 11 Sirocco fan installed near the Colorado shaft, provided the Colorado mine with a maximum of approximately 30,000 cu. ft. per min. of relatively fresh air, most of which came in a fairly direct route from the downcast Belmont shaft through the No. 11 fan to the 2500-ft. level stopes. After passing through these stopes and the stopes of overlying levels, it passed through the main crosscuts on higher levels back to the Colorado shaft, which provided the upcast for this current of air. The improvement

Jan 9, 1921

By T. M. Williams

DURING the year just ended we have had three great fires in the mines in the Wilkes-Barre district. One at the Empire Colliery, one at the Prospect shaft, and the other at the Baltimore old mine. It is proposed in this paper to give a brief history of the fire at the Empire Colliery, and the methods employed in extinguishing it. The fire was first discovered breaking out in the air-stack, alongside what is known as the " Kidder Plane," about one o'clock on the morning of December 31st, 1873. Subsequently it was ascertained that the fire originated in the return airway somewhere near the steam boiler, located inside the mine, near the head of No. 5 slope. The coal from this slope was hoisted to the shaft gangway, at a point nearly four thousand feet distant from the foot of the shaft. As there were from four to five hundred mine cars hoisted per day from this slope the steam boilers were located at this place. The mines being of considerable extent required a large volume of pure air for ventilation, and no fan having been erected at this slope at the time, the heat from the boiler was made use of to assist ventilation, by conveying the return air from No. 5 slope into the large airway made from these boilers to the surface through the old "Kidder slope" to the stack where the fire was first discovered. The length of this slope or airway was about one thousand feet, with a sectional area of about sixty feet. The quantity of air passing through it must have been over sixty thousand cubic feet per minute

Jan 1, 1875