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By R. A. Haney, S. J. Gigliotti

Over the past ten years, analysis of the acceptability of face ventilation systems has been based on numerical criteria rather than solely a study of air flow and methane patterns in the face area. This type of analysis has become possible primarily because of the instrumentation and mathematical models developed by the Ventilation Division, Pittsburgh Health Technology Center, Mine Safety and Health Administration (MSHA). To properly use these mathematical models, large amounts of methane and airflow data must be collected in the face area during mining activities. To supplement underground testing of face ventilation systems, a full scale model of a face area was built. This model includes a full scale model continuous miner, a face ventilation system, a gas release system, and a remote methane detection system. The remote methane detection system consists of an array of twelve methane sensors located throughout the face area. Data from the sensors are transmitted to strip chart recorders. Methane, air quantity, and other data collected during a test are entered into a computer for analysis. This paper presents the data entry system, the models used for data analysis, the test results, and the application of these results to a face ventilation system.

Jan 1, 1983

By K. F. Unrug

Eastern coalfields have been extensively strip mined. In the past, contour mining left vast areas of post-mining highwalls and benches. Thin seams, which cannot be feasibly mined with conventional methods, quite often contain substantial reserves of high quality coal. Unconventional secondary recovery methods may permit economical production of that coal, increased use of reserves, and provide resources for restoration of orphaned land. Technical and rock mechanics implications of secondary mining methods are discussed to determine their limitations and the objectives of required research.

Jan 1, 1986

By Ian William Wark, Keith Leonard Sutherland

MERCAPTOBENZTHIAZOLE and its sodium salt are marketed under the trade names Flotagen and Flotagen S respectively, for use as collectors for cerussite and other minerals. The structural formulas for sodium mercaptobenzthiazole and for sodium ethyl xanthate are: [ ] Chemically there is a resemblance between the two compounds, though the free acid (mercaptobenzthiazole itself) is much more stable than xanthic acid. Both are readily oxidized, e.g., by iodine to disulphides, and can be estimated by iodometric titration. Qualitatively they are similar as collectors in flotation, although there are quantitative differences between them that may be important in practice. It is deduced that the influence of the nitrogen atom is subordinated to that of the sulphur atoms, and that the dominant group of these compounds is the mercapto group -SH or -SNa. The general method of investigation has been based on contact tests. Two temperatures, 10º and 35º C., have been chosen, and with a standard concentration of 20 mg. per liter of mercaptobenzthiazole (i.e., of the free acid) the influence of alkali, cyanide and copper sulphate on contact at sulphide mineral surfaces has been studied. This standard concentration corresponds to about 19 mg. per liter potassium ethyl xanthate; it brings out the differences between the minerals better than a higher concentra-

Jan 1, 1939

By Albert R. Ledoux

I am indebted to The Kaolin Co. of West Cornwall, Conn., and particularly to its engineer, Mr. M. Wanner, for permission to make public, through the Transactions of the American Institute of Mining Engineers, the interesting results of his experiments, having in view the winning of kaolin from deep deposits without shaft-sinking or removing of the overburden. So far as I am aware, nothing like it has been accomplished heretofore, although it reminds one of the methods successfully employed in Louisiana for the winning of sulphur from deep beds by the sinking of pipes one within another, injecting superheated steam under pressure through one pipe, the heat of the steam liquefying the sulphur and the pressure forcing it up through the other pipe to bins at the surface. The kaolin-deposit at West Cornwall is an alteration in situ— that is, it is not sedimentary. A series of clay-veins, dipping about 50" from the vertical, lie between a foot-wall of' limonite and a hanging-wall of gneiss and hornblende schist. The clay-veins alternate with veins or seams of more or less broken quartz, and unaltered feldspar. The deposit, which occurs at a point about 600 ft. above the Housatonic river, was opened five years ago, and about 5,000 tons of a superior grade of washed kaolin have been extracted from open pits, and sold. It soon became evident that this mode of extracting the product would prove unremunerative, by reason of the dip of the vein and the intercalary strata and lenses of quartz, and a more satisfactory method of working the deposit was sought. It is well understood that, in the preparation of all clays for market, especially residuary kaolin, the most important as well as the most difficult step is the washing of the crude product. The dificulties increaee with the percentage of foreign matter, especially quartz and mica, contained in the product. Hence, a system

Jan 1, 1907

By F. R. Wadleigh

It is generally realized and very often admitted by both producers and consumers of coal that there is great need for a revision of existing commercial classifications, and this will involve, of course, determination of a standard classification and a constant revision of marketing practices as they are affected by coal classification. I recently sent out some 200 letters to producers and consumers with a request for their views on the subject of commercial classification. Nearly all of the replies from both sides were that there was needed some change in the present method. There were three or four dissenting voices but the great majority of opinion was in favor of the formulation of some standard commercial classification. The classifications in commercial use today can best be described as a hodgepodge. They are made upon different bases, have different names and have different ways. There are, for instance, about 11 single bases of classifications as used commercially and some 17 or 18 combination bases. Then there were the Tidewater Pool Exchanges. The classification which they put in force is still used in the tidewater markets and has several different bases of its own. It will be considerable of an undertaking to bring about a change in marketing methods as affected by coal classification but it is well worth doing and I think the committee which has been appointed under the auspices of the American Society for Testing Materials realizes the importance of the subject and is on the way to at least bring about some provision for adjusting matters. By way of starting, each member of the Committee on Commercial Classification has been assigned to a general market district and each member is now engaged in collecting the commercial market practice data for submission at the next meeting of the Committee. About a year ago I made up a list of the commercial classifications in the different markets and the total was 171. The 11 single bases I found used in commercial practice were:

Jan 1, 1930

By A. W. Faheneald, Lewis S. Prater

By taking advantage of the fundamental difference between screening and classification—namely, that specific gravity has no effect on screening but is one of the important factors in classification—a combination of the two may be used as a process of mineral concentration. Although this fact is not new, so far as is known it has had little or no commercial application. The scheme is not presented now as a process for producing finished products but rather as a preliminary operation rejecting part of the barren material from an ore before it is subjected to more costly treatment. That is largely the function of the new heavy-media concentration processes that have been widely accepted. Original installation costs for the present sink-float processes are relatively high, however, which confines their use to operations where large tonnages are handled. Sink-float has been successful on only the relatively coarse (approximately plus 10-mesh) portion of an ore, and it is in this same range that classification screening can function most satisfactorily. Theoretically, there is no upper limit to the size of particles that can be handled in a sink-float operation, but the degree of liberation in the very large pieces usually limits this. With classification screening, particles from % to % in. would be the largest that could be handled, but the lower range could be extended somewhat below 10 mesh. In order to take full advantage of the difference in specific gravities of the minerals being separated, sorting in the classifier should be under as extreme hindered-settling conditions as possible. Laboratory tests have been made on a galena ore and on an artificial mixture of quartz and magnesite to determine the separations that may be expected. Although more than one scheme may be followed, in these tests the separations were made by cutting the underflow from the classifier as a concentrate and then screening the overflow. The screen oversize was rejected as a tailing. Classification was done in a hindered-settling teeter column and screening was done by hand, using the standard 4 2 series. The accompanying flowsheet gives the testing procedure followed.

Jan 1, 1947

By A. W. Faheneald, Lewis S. Prater

By taking advantage of the fundamental difference between screening and classification—namely, that specific gravity has no effect on screening but is one of the important factors in classification—a combination of the two may be used as a process of mineral concentration. Although this fact is not new, so far as is known it has had little or no commercial application. The scheme is not presented now as a process for producing finished products but rather as a preliminary operation rejecting part of the barren material from an ore before it is subjected to more costly treatment. That is largely the function of the new heavy-media concentration processes that have been widely accepted. Original installation costs for the present sink-float processes are relatively high, however, which confines their use to operations where large tonnages are handled. Sink-float has been successful on only the relatively coarse (approximately plus 10-mesh) portion of an ore, and it is in this same range that classification screening can function most satisfactorily. Theoretically, there is no upper limit to the size of particles that can be handled in a sink-float operation, but the degree of liberation in the very large pieces usually limits this. With classification screening, particles from % to % in. would be the largest that could be handled, but the lower range could be extended somewhat below 10 mesh. In order to take full advantage of the difference in specific gravities of the minerals being separated, sorting in the classifier should be under as extreme hindered-settling conditions as possible. Laboratory tests have been made on a galena ore and on an artificial mixture of quartz and magnesite to determine the separations that may be expected. Although more than one scheme may be followed, in these tests the separations were made by cutting the underflow from the classifier as a concentrate and then screening the overflow. The screen oversize was rejected as a tailing. Classification was done in a hindered-settling teeter column and screening was done by hand, using the standard 4 2 series. The accompanying flowsheet gives the testing procedure followed.

Jan 1, 1947

By Robert Berggren

THE hot-milling process for reconditioning rock-drill bits is not new. It has been employed by a few mines for years and in the past decade it has been widely adopted, as its advantages have become better known. Because of the extensive commercial development in England and Canada of machines to operate on this principle, general acceptance has been largely in the British possessions and until recently has been chiefly in the field of conventional steel. In the past two years there has been a definite trend toward hot-milling of detachable bits in Canada, t but only in the past year has any considerable attempt been made to build special machines for this type of work. Generally a machine designed for con-ventional steel has been used and special holders employed to manipulate the bit. As early as 1934 at least one operator in the United States had adapted hot-milling to conventional steel with a substantial saving in resharpening costs. Several other operators have taken it up but there has been no widespread adoption of the method in this country by users of conventional steel. This may be partly explained by the fact that until recently no American manufacturer produced this equipment and operators have been obliged to build their own hot-millers or import them. Several years ago a few machines were built in Seattle, Wash-ington, and operated in some mines in the northwest, but, for reasons not generally known, the effort was abandoned.

Jan 1, 1940

By T. Sterry Hunt

IN my address on the " Geognostical Relations of the Metals," delivered before the Institute on the 20th of February last (Vol. I Transactions, p. 331), I spoke of the rocks in the vicinity of Thunder Bay, Lake Superior, where I indicated two series of uncrystalline rocks resting upon the Huronian schists, the lower one consisting of dark-colored argillites and sandstones overlaid, apparently in slight discordance, by nearly horizontal red and white sandstone and marls, which were compared with those of Sault Ste. Marie, and those of the Portage Lake district, on the south shore. These latter sand-stones, according to Brooks and Pumpelly, overlie unconformably the Keweenaw series of copper-bearing amygdaloids, sandstones, and conglomerates, and are in turn overlaid by the Trenton limestone. I then proposed to call this lower series of Thunder Bay, that is to say, the dark-colored argillites and sandstones which are traversed by the silver-bearing lodes of that region, the Animikie group. Shortly after the publication of that address I received an abstract of a paper on the geology of that region by Professor Robert Bell, read before the Montreal Natural History Society, February 24th. He there confirms the statement made in my address that the gold of Lake Shebandowan occurs in the Huronian, which is also seen to be cut by the silver-bearing lodes just mentioned. Professor Bell, in this paper, proposes to designate both what I have called the Animikie group, and the overlying red and white sandstones, by the name of the Nepigon group, for the reason that the upper series is best displayed about Lake Nepigon. This latter series is by Logan supposed to be overlaid by the copper-bearing amygdaloids with conglomerates and sandstones of the north shore (apparently identical with those of Keweenaw) ; and the whole together, including the Animikie group, constitute his Upper Copper-bearing group. These copper-bearing strata are by him supposed to be overlaid by the red and white sandstones of St. Mary, which are apparently the same with those sandstones which, according to Brooks and Pumpelly, overlie unconformably the similar cupriferous rocks of Portage Lake, and are, in their turn, overlaid by the Trenton limestone. Thus the sandstones which at Thunder Cape overlie the Animikie group are by Logan placed in the midst of the Upper Copper-bear-

Jan 1, 1874

By D. J. McAdam, G. W. Geil, R. W. Mebs

As shown in previous papers by the authorsg-17t the resistance of a metal to fracture, like its resistance to plastic deformation, is a function of all three principal stresses. A technical cohesion limit is the technically determined resistance to fracture under a specific stress system. The technical cohesive strength thus comprises an infinite number of technical cohesion limits corresponding to the infinite number Of possible com-binations of the principal stresses. The technical cohesive strength, therefore, may be represented by a surface in a diagram with the three principal stresses as coordinates. As shown in previous papers,'-'' the technical cohesive strength increases with plastic deformation, with decrease in temperature, and with increase in the strain rate. The technical cohesion limit, therefore, is affected by the same factors that affect the flow stress,$ namely, the stress system, plastic deformation, temperature, and the strain rate. More- over, the influence of each of these factors on the technical cohesion limit has been shown to be qualitatively similar to the three of the same factor on the flow stress.9-18 Advance of knowledge about the conditions determining fracture of metals has been retarded by the reluctance of some investigators to abandon preconceived ideas about how metals ''should,, behave. The incorrect idea is still prevalent that the conditions determining resistance to fracture are very different from those determining the flow stress. Attempts are still being made to express resistance to fracture in terms of a single parameter, such as a limiting value of the greatest principal stress, the maximum shearing stress, or the volume stress (one-third the algebraic sum of the three principal stresses). In these attempts, a sharp distinction is sometimes made between a ductile or ,plasticdeformation, fracture,, and a "brittle frat-ture.H In making this distinction, however, the meaning attached to the term "brittle fracture" sometimes is not made clear. The term could mean fracture after very little plastic deformation or it could be used to designate the type of fracture. An ordinary fracture of a ductile metal at room temperature starts as a cleavage, generally transverse to the direction of the greatest principal stress, but eventually changes to a shearing fracture' In some conditions, however, the metal fractures entirely by cleavage, with no evidence of plastic deformation during the fracture; the surface of such a fracture may have a

Jan 1, 1948

By R. W. Mebs, G. W. Geil, D. J. McAdam

As shown in previous papers by the authorsg-17t the resistance of a metal to fracture, like its resistance to plastic deformation, is a function of all three principal stresses. A technical cohesion limit is the technically determined resistance to fracture under a specific stress system. The technical cohesive strength thus comprises an infinite number of technical cohesion limits corresponding to the infinite number Of possible com-binations of the principal stresses. The technical cohesive strength, therefore, may be represented by a surface in a diagram with the three principal stresses as coordinates. As shown in previous papers,'-'' the technical cohesive strength increases with plastic deformation, with decrease in temperature, and with increase in the strain rate. The technical cohesion limit, therefore, is affected by the same factors that affect the flow stress,$ namely, the stress system, plastic deformation, temperature, and the strain rate. More- over, the influence of each of these factors on the technical cohesion limit has been shown to be qualitatively similar to the three of the same factor on the flow stress.9-18 Advance of knowledge about the conditions determining fracture of metals has been retarded by the reluctance of some investigators to abandon preconceived ideas about how metals ''should,, behave. The incorrect idea is still prevalent that the conditions determining resistance to fracture are very different from those determining the flow stress. Attempts are still being made to express resistance to fracture in terms of a single parameter, such as a limiting value of the greatest principal stress, the maximum shearing stress, or the volume stress (one-third the algebraic sum of the three principal stresses). In these attempts, a sharp distinction is sometimes made between a ductile or ,plasticdeformation, fracture,, and a "brittle frat-ture.H In making this distinction, however, the meaning attached to the term "brittle fracture" sometimes is not made clear. The term could mean fracture after very little plastic deformation or it could be used to designate the type of fracture. An ordinary fracture of a ductile metal at room temperature starts as a cleavage, generally transverse to the direction of the greatest principal stress, but eventually changes to a shearing fracture' In some conditions, however, the metal fractures entirely by cleavage, with no evidence of plastic deformation during the fracture; the surface of such a fracture may have a

Jan 1, 1948

By Arthur Lubinski, K. A. Blenkarn

It is explained why the bottom portion of freely suspended tubing in a pumping well buckles and straightens in succession during the pumping cycle. Field evidence of resulting rod-on-tubing wear, excessive polished rod load, and excessive horsepower are given. The possibility that buckling hastens pump wear is strongly suggested. Means for either prevention of buckling or for mini-mizing its effects are explained, their relative merits compared, and field results of their use given. These means are: tension anchors, tail pipe, sucker rod guides, and corrosion inhibitors. Charts and formulas for best use of tension anchors, tail pipe, and guides are given. Use of tension anchors, or compression anchors with a heavy tail pipe, prevents both buckling and breathing, thus improving volumetric efficiency. Without tail pipe, buckling above compression anchors precludes such improvement. INTRODUCTION It is well known that a column must be subjected to some compression in order to buckle; and also that a structural member does not buckle if subjected to a tension. When consideration is given to a tubular column, the question may be asked, "How is the buckling phenomenon affected by inside or outside pressure?' At first, it seemingly should not be affected. However, this is not so. In order to arrive at a correct deduction one should first understand the basic reasons for buckling of a column under loading*. Then he should add to the effect of that loading the effect of pressure. Following this procedure, one may discover quite unexpected phenomena. In some cases, when subjected to more pressure inside than outside, a pipe may buckle under tension. In other cases, a pipe may remain straight, although subjected to a very large compression. In 1950 and 1951 it was explained why the bottom portion of a string of pipe freely suspended in a well does not buckle even when subjected to a large compression due to buoy- ancy.2,3 It was shown that the com-monly used concept of a neutral point, as being a point in the string with neither compression nor tension, is inadequate, and a more relevant definition of the neutral point was introduced. The findings were also generalized to cases of different pressures inside and outside a pipe.3a Later, in a further generalization, allowance was made for variations of stress and pressure with depth.' The findings were applied to the new technique of hydrostatic high pressure testing of lengths of pipe in the mill.5 In 1952 it was observed that previous theoretical findings apply to tubing in pumping wells. The lower part of freely suspended tubing buckles during the upstroke portion of the pumping cycle. Later, it was ascertained that this phenomenon is responsible for wear and malfunctioning of the equipment. Various remedial measures were devised and successful field trials conducted. Only brief mentions on the subject have been published.6,7 In this paper, the phenomenon of tubing buckling is explained, field

Jan 1, 1958

By J. Lewis, J. Harper, M. F. Ashby

A grain boundary in a metal interacts with second-phase particles, which exert a pinning force (first estimated by Zener) on the boundary opposing its motion. We have computed the shape of boundaries which interact with more or less spherical second-phase particles and have constructed a soap-film model to reproduce the shape of the boundary surface. An important result is that measurement of this shape allows the pressure, or driving force, on the boundary to be measured. We hare applied this technique to grain boundaries in two alloys and hate measured the pinning force exerted by single second-phase jwrticles on the boundaries. It is in good agreement with Zener's estimate. J\. boundary between two grains, or two bulk phases, interacts with small inclusions or particles of a second phase, whether they are gas or solid. This interaction means that the boundary, forced to migrate by a difference in free energy between the material of the two grains or phases which it separates, exerts a force on a particle which it touches, tending to drag it forward. (The movement of inclusions through metals under the influence of this force, has, in fact, been observed. 1-3) Equally, the particle can be thought of as exerting a pinning force on the boundary, tending to hold it back. Zener (in a celebrated private communication4) first realized that this interaction, and the resulting pinning force, existed. His calculation of its magnitude was crude but adequate: a spherical inclusion of radius r blanks off an area nr2 of the boundary on which it sits; since the boundary has an energy of rMM x per unit area, the blanlung-olf decreases the energy of the system by MM: this energy is returned to the system if the boundary is pulled free from the inclusion— a forward movement of the boundary by a distance r will do this—so that the maximum pinning force is Trrym.M- A similar argument can be made for inter-phase boundaries. The nature of the particle itself did not enter this, or two subsequent treatments.5,6 When it is considered, tic leifthe energyoftheb a) The boundary may enter and pass through the particle if the energy of the boundary is lower within the particle than in the matrix. Fig. l(r/). Certain coherent precipitate particles behave like this. h) More usually, the boundary will bend round the particle, enveloping and bypassing it. Fig. l(b). In doing so, it changes the structure and energy of the interface between the particle and its matrix. This means that the boundary does not touch the particle surface at right angles, as early treatments assumed,5'9 but at some angle a which depends on this change in surface energy of the particle, and can be calculated from the equilibrium of surface tensions. Most precipitate particles and inclusions behave like this. Gas bubbles or liquid drops can be regarded as belonging to either group. The progress of bypassing is conveniently measured by the angle shown in Fig. 1. When the nature of the particle is ignored, its maximum pinning force is exerted when - 45 deg. When it is considered, this critical value of is found to depend on a and thus on the nature of the particle. The maximum pinning force lies between nryMM and 2jtjMM (Appendix 1). not very different from Zener's result. In reality, a boundary between crystals has a specific energy and tension which varies with the orientation of the boundary. Furthermore, recent experiments7 indicate that such a boundary is not atom-ically smooth, but has steps on it: migration of the boundary corresponds to the sweeping of these steps across the boundary surface, like the Frank model of crystal growth from the vapor. This means that the interaction of a boundary with particles should really be considered in terms of the way in which particles hinder the movement of these steps. To suppose a grain boundary or interphase boundary to be smooth, and to ignore the variation of its energy with orientation, is to liken it to a soap film. The advantage of this soap film approximation, which we have used throughout this paper, is that interaction energies and boundary shapes can be calculated easily. We have done this by numerical computation and by using a soap film model, and have compared the results with grain boundaries in an aluminum-based and a copper-based alloy. It turns out that the shape of the boundary which bulges between particles allows the pressure an it to be calculated; that is, the local driving force an the boundary can be measured. This has allowed us to check the Zener relationship experimentally.

Jan 1, 1970

By R. G. Aspden

Crystals with an (001) [loo] initial orientation of an iron-base alloy containing 3 pct Si were cold rolled with and without the use of constraints. A major difference in the rolling and annealing textures was observed between crystals rolled with and without constraints. These data show that the contribution of constraints at grain boundaries in a poly crystalline sheet should be considered in applying textural data on single crystals to grains in an aggregate. SILICON-iron alloys with a cube texture have been recently developed and their magnetic characteristics reported.1-4 Of interest in the development of this texture were the textural changes of single crystals accompanying rolling and annealing and the influence of constraints at grain boundaries in an aggregate on the behavior of individual grains. The present study was primarily concerned with the effect of constraints during rolling on the textures of 3 pct Si-Fe crystals initially (001)[100]. Barrett and Levenson5 were among the first to observe an influence of constraints at grain boundaries on the textural changes of individual grains during deformation. They tested Taylor's6 theory of plastic deformation of face-centered-cubic metals in which deformation textures were predicted. About one-third of the grains in poly crystalline aluminum did not rotate as predicted. Grains of the same initial orientation were observed to rotate in different directions under the influence of applied stress and anisotropic flow of neighboring grains. Recently, the various inhomogeneities of flow of crystals in an aggregate have been studied7'8 and reviewed.9-11 Barrett and Levenson" rolled (001) [loo] iron single crystals inserted in close-fitting holes in copper to limit lateral flow and to simulate rolling of grains in an aggregate. Deformation bands were formed after a 90 pct reduction in thickness, and the cold-rolling texture contained two components described by rotating the (001)[100] about 35 deg in both directions around the normal of the rolling plane. No annealing textures were reported. Chen and Maddin13 rolled molybdenum single crystals initially (001) [loo]. The crystals were mounted between two hardened silicon-iron plates and 96 pct reduced in thickness by rolling at a low rate of reduction, about 0.0001 in. per pass. The deformation texture had the mean orientation of (001) [loo], and the azimuthal spread included orientations described by rotating (001) [loo] about 35 deg in both directions about the pole of the rolling plane. The presence of deformation bands were not reported by Chen and Maddin or detected in subsequent work of Ujiiye and Maddin.14 The ideal orientation of the annealing texture was (001) [loo]. Recently, Walter and Hibbard 15 reported on the textures of 3 pct Si-Fe alloy crystals initially near (001) [loo]. Each crystal was in an aggregate cut from a columnar ingot. After 66 pct reduction by rolling, the texture consisted of two symmetrical components which had the orientations described by rotating (001) [loo] about 30 deg in both directions about the pole of the rolling plane. Annealing texture was near (001) [loo]. In the above work, the textures of body-centered-cubic crystals were studied after rolling under the influence of constraints. The deformation textures varied from (001) [loo] to near the (001) [110] type and appeared sensitive to the manner in which the crystals were rolled. No textural data were available on the effect of rolling (001) [loo] crystals with and without constraints. The purpose of the present work was to evaluate the influence of constraints during rolling on the textures of 3 pct Si-Fe crystals initially (001) [loo]. Rolling and annealing textures were studied for a) crystals rolled with no constraints at different rates of reduction, and b) crystals rolled with constraints imposed by neighboring grains and by plates between which a crystal was "sandwiched". PROCEDURES AND EXPERIMENTAL TECHNIQUES Data are presented on four crystals which are representative of several crystals studied. The orientation of each crystal prior to rolling was (001) [loo] as determined by the Laue X-ray back-reflection method," i.e., each crystal had an (001) within 3 deg of the rolling plane and [100] within 3 deg of the rolling direction. These crystals were obtained from two iron-base alloys containing 3 pct Si by weight which were prepared by vacuum melting electrolytic iron and a commercial grade of silicon. Crystals 1, 2, and S-1 were cut from a large single crystal grown from the melt of one alloy by the Bridgman technique17 in an apparatus described by

Jan 1, 1960

By N. Mungan

Formation damage, i.e.. reduclion in permeability, has been generally attribuled to clay minerals which expand or disperse upon contact with water that is less saline than the connate water. Luboratory, studies show that penneahility reduction can also occur in formalions containing only nonexpandable clays such as illite or kaolinite, and can be caused also by changes in pH. Furthermore, pH changes can damage even formations that are essentially free of clays. It is suggested that permeability reduction is due to the small passages being blocked by particles, which may be dispersed clays, cemenlion material or other fine parricles. These particles are dislodged by dispersion of clays due to changes in salinity or by dissolution of calcareous cement by acids, or of silicaceous cement by alkaline solutions. In working with reservoir cores, it was found that extracted cores damaged more easily and extensively than nonextracted cores. The extent of damage depended also on tenlperatltre. INTRODUCTION Permeability is an important property of porous media and has been the subject of many studies by engineers and geologists. Many of these studies are conccrned with formation damage, i.e., reduction in permeability, resulting from exposure of oil-producing formations to water substantially less saline than the connate water. This effect causes understandable concern since during drilling, completion and production phases formations are often exposed to fresh water. The damage resulting from contact with relatively fresh water has been attributed to expansion and dispersion oF clay minerals. During laboratory investigation of the use of NaOH as a wettability reversal agent to increase oil recovery from oil-wet reservoirs, several cores used in the displacement studies suffered loss in permeability. Despite the traditional usage of NaOH for conditioning aqueous mud systems, the role of the caustic filtrate in wellbore damage seems to have been overlooked. Browning2 as recently reported on the effects of NaOH in dispersing clay minerals but he was concerned only with complications that may arise in drilling massive shale beds. The following study was made to examine the role of pH and salinity changes in core damage. Where cores from reservoirs were used, tests were performed with extracted and nonextracted cores both at room and reser- voir temperatures, since it was felt that the test environment and core condition may affect the results. Because of its limited coverage and exploratory nature, this study is not intended to provide answers to field formation damage problems. It is hoped that it will encourage research into new aspects of the permeability reduction problems, particularly those allied to new recovery and production processes. PROCEDURE In all permeability tests, fluids were pumped through the cores at a constant volumetric rate. Only deaerated fluids and reagent grade chemicals were used. The fluids were passed through two ultrafine filters before injection to remove any entrained particles. The cores, with the exception of the unconsolidated cores, were mounted in Hassler holders. Water was used to transmit pressure to the sleeve. The inlet endpiece had two entry ports which permitted scavenging one fluid with another to avoid any mixing in the small holdup volume. The cores were flushed with CO2 gas, evacuated for 5 to 6 hours and saturated with the first liquid at a pressure of 1,000 psi for 24 hours to eliminate any free gas from the cores. Pressure differences up to 20 psi were measured by transducers, calibrated in inches of water and continuously recorded. For greater pressure drops, gauges were used. All reservoir cores were cleaned with a light refined mineral oil, then with heptane, and finally dried with CO2. Compatibility tests showed that no precipitates formed when mineral oil and the crudes were mixed. Some cores were extracted in Dean-Stark-type solvent extractors using xylene and trichloroethane and dried in a vacuum oven at 450F. Each test consisted of a sequence of water, test solution, and again water flow. RESULTS AND DISCUSSION STUDIES IN BEREA CORES Salinity Contrast Berea cores 2-in. in diameter and 12-in. long were cut from sandstone quarried in Cleveland, Ohio. The clay minerals were identified by X-ray diffraction to be chlorite, kaolinite, illite and incerlayered illite. Flow of fresh water or 30,000 ppm brinc does not cause any permeability reduction (Fig. 1). However, after injection of brine the core is readily damaged by fresh water. Damage starts almost instantly as the fresh water injection is begun, and at a cumulative injection of 1.2 PV fresh water, the permeability has dropped from 190 to 0.9 md. Upon continued injection, the effluent contains clay minerals dislodged from the core. The final core per-

Jan 1, 1966

By S. C. Sun, John A. L. Campbell

The surface properties exhibited by bituminous coal and bituminous coal lithotypes were ascertained by using streaming potential techniques. The electro kinetic prop-erties wereascertainederties of bituminous coal were found to be similar to those of anthracite. The principle electrokinetic properties of the coal and lithotypes, zero-points-of-charge (ZPC), and potential determining ions, were established. The effects of indifferent electrolytes, hydronium and hydroxyl ion sources, and polyvalent ions (cationic and anionic) were also evaluated. Location of the ZPC's with respect to pH is discussed in terms of chemical and mineralogical composition of the respective surfaces. To account for the observed electrokinetic phenomena, a generalized surface model and adsorption mechanism are proposed. Surface-dependent processes, such as froth flotation and flocculation, are important or potentially important techniques for combating some of the current major problems in coal preparation. In order to correctly apply or improve a surface-dependent process, it is of paramount importance to understand the interfacial phenomenon, especially the double layer properties, exhibited by the solid. The specific objective of this research was to determine the properties of the bituminous coal/liquid interface by an electrokinetic method, streaming potential, and to relate the findings, wherever possible, to the existing unit operations of froth flotation and floccula-tion tion. The electrokinetic properties of both the whole coal and its lithotypes were investigated. As part of the total investigation, the role played in the double layer by the reagents commonly employed in the surface dependent process was also established.' These data will be presented at a later date. Experimental Procedures The coal samples used in this research and their designations are listed in Table 1. The classical description of humic coal lithotypes as developed by Stopes" was used for the delineation of the lithotype samples. The samples were taken from the working face of a producing deep mine of the Pittsburgh seam in the area of Ellsworth, Pa. To avoid oxidation, only freshly exposed areas were sampled. The normal precautions against contamination were also exercised. Two types of samples were taken, specimens rich in a particular lithotype and a representative channel sample. The latter sample was prepared for analyses by grinding it to —35 mesh. It was screened repeatedly during the grinding to provide the largest amount of 35 x 48-mesh (standard Tyler sieves) material possible. The screened fraction was passed over a magnet and then washed several times with distilled water and finally with conductivity water. The resulting sample now termed "whole coal" was stored under conductivity water in a glass bottle. Pure lithotypes were obtained from the lithotype concentrates by hand picking, and were processed in the same manner as the representative sample. Maceral analyses, employing standard petrographic procedures," were performed on the lithotype samples to determine the purity of the samples. The results are presented in Table 2. Reflectance measurements of the vitrinites and fusinites are also reported in this table. Proximate and ultimate analyses of the samples are given in Tables 3 and 4. The electrokinetic properties of the coal samples were determined by streaming potential methods.'-' All of the chemicals used in the investigation were reagent grade (Baker analyzed). The conductivity water was prepared by doubly distilling the water in a pyrex Yoe-type still and passing the distillate through a mixed bed ion exchange column. Results In general, the electrokinetic properties of the investigated bituminous coal were found to be similar to the results of a previous study of anthracite by Camp-bell bell5 and are in accord with the suppositions of Brown." The zeta potentials of the coal and all the lithotypes were found to be negative in conductivity water. Jowett? in a study of slime coatings on coal also found bituminous coal to exhibit a negative surface. Fig. 1 shows that the negative charges, at neutral pH's, for both fusain and the gangue are very small, almost zero, while at the same pH, vitrain has the largest negative charge, almost 30 mv. Durain has a negative charge of 17.5 mv. The determination of the affect of pH on the charge of the coal surfaces revealed that hydronium and hydroxyl ions apparently behave as potential determining ions; however, they do not appear to be potential determining for the gangue. These results are illustrated in Fig. 1. As the pH of the solution was decreased, hydronium ions were adsorbed, causing the surface of the coal to reverse polarity and become

Jan 1, 1971

By Vittal S. Bhandary, B. D. Cullity

Swaged iron wire has a cylindrical {001} <110> texture. The texture is also cylindrical after re-crystallization in the absence of a magnetic field, but <111> and <112> components are added to this texture when recrystallization occurs in a field. The mecizanical properties in tension and in torsion are not greatly altered by these changes in texture. AS shown in a previous paper,1 cold-worked wires of the two fcc metals copper and aluminum can be made relatively strong in torsion and weak in tension, or vice versa, by proper control of preferred orientation (texture). The deformation texture can be controlled by selection of the starting texture (texture before deformation), because certain initial orientations are stable during deformation. The present paper reports on similar work performed on bcc iron. In this case it was clear at the outset that there was no hope of controlling the deformation texture, which is one in which <110> directions are aligned parallel to the wire axis. (1t has usually been regarded as a fiber texture, but Leber2 has recently shown that it is a cylindrical texture of the type {001} <110>. In either case, <110> directions are parallel to the wire axis.) There is general agreement on this texture among a large number of investigators, which in itself suggests that the starting texture has no influence on the deformation texture. More direct evidence was produced by Barrett and Levenson,3 who reported that iron single crystals of widely varying initial orientations all had a single <110> texture when cold-worked into wire. Thus <110> is a truly stable end orientation for iron and probably for other bcc metals as well. Under these circumstances attention was directed to the possibility of controlling the recrystallization texture. This texture is normally <110> in iron,4 just like the deformation texture. However, it is conceivable that this texture could be modified by a proper choice of the time, the temperature, and what might loosely be called the "environment" of the recrystallization heat treatment. In the present work the environmental factor studied was a magnetic field. The effect of heating in a magnetic field ("magnetic annealing") on recrystallization texture has been investigated by Smoluchowski and Turner.5 They found that a magnetic field produced certain changes in the recrystallization texture of a cold-rolled Fe-Co alloy. The texture of this material is normally a mixture of three components, and the effect of the field was to increase the amount of one component at the expense of the other two. Smoluchowski and Turner concluded that the effect was due to magnetostriction. With the applied field parallel to the rolling direction, the observed effect was an increase in the amount of the texture component which had <110> parallel to the rolling direction. In the Fe-Co alloy they studied, the magnetostriction is low in the <110> direction and high in the <100> direction. Thus nuclei oriented with <110> parallel to the rolling direction will have less strain energy than those with <100> orientations and will therefore be more likely to grow. In a later paper on the same subject, Sawyer and Smoluchowski6 ascribed the effect to magneto-crystalline anisotropy and made no mention of magnetostriction. In the papers of Smoluchowski et al. the intensity of the magnetic field was not reported but it was presumably large, inasmuch as it was produced by an electromagnet. In the second paper6 it is specifically mentioned that the specimens were magnetically saturated. But if magnetostriction has a selective action on the genesis of stable nuclei during recrystallization, that selectivity must depend only on differences in magneto-strictive strains between different crystal orientations and not on the absolute values of those strains. Thus the saturated state does not necessarily produce the greatest selectivity, because the relative difference in magnetostrictive strains between different crystal directions may be larger for partially magnetized crystals than for fully saturated ones.7 In the present work the specimens were subjected to relatively weak fields (0 to 100 oe) produced by solenoids. MATERIALS AND METHODS Armco ingot iron rod (containing 0.02 pct C and 0.19 pct other impurities) was swaged from 0.25 in. in diam. to 0.05 in., a reduction in area of 96 pct. The mechanical properties in tension and torsion were measured as described previously.&apos; Textures were measured quantitatively with chromium or iron radiation and an X-ray diffractometer,8,1 and

Jan 1, 1962

By M. D. Arnold, H. J. Gonzalez, P. B. Crawford

A method is presented for estimating the effective directional permeability ratio and the direction of maximum and minimum permeabilities in anisotropic oil reservoirs. The method is based on the principle that production from a well in an anisotropic reservoir results in elliptical isopo-tentials about the well, rather than circular. Bottom-hole pressure data from three observation wells surrounding a producing well are required to apply the method. The method involves fitting field pressure data to a set of general charts of isopotentials and making a few simple calculations until a solution is found. The method is based on a steady-state equation for homogeneorrs fluid pow. In addition to the method, a brief discussion of the theory underlying it is presented. INTRODUCTION The existence of a different permeability in one direction than another in oil reservoirs has been mentioned in several papers. Hutchinson&apos; reported laboratory tests on 10 limestone cores and pointed out that one-half of them showed significant, preferential, directional permeability ratios, the average being about 16:1. Johnson and Hughesz reported a permeability trend in the Bradford field in the northeast-southwest direction with flow being 25 to 30 per cent greater in that direction. Barfield, Jordan and Moore -eported an effective permeability ratio of 144:1 in the Spraberry. Crawford and Landrum4 showed that sweep efficiencies could often vary by a factor of two to four, and sometimes considerably more, due to variations in flooding direction and patterns in anisotropic media. These findings indicate that the poss&apos;bility of anisotropy may be worthy of consideration in the development of an oil field. In considering this, it should first be determined if anisotropy exists. If it does, the direction of the maximum and minimum permeabilities and the ratio of their magnitudes are quantities which can be of value in planning the most efficient well-spacing patterns. Past methods of determining these quantities have included analysis of oriented cores and analysis of flooding performance of pilot injection patterns. In recent work, Elkins and Skov5 resented an analysis of the pressure behavior in the Spraberry which accounted for anisotropic permeability. This work was based on the transient pres- sure distribution in a porous and permeable medium, with the solution expressed as an exponential integral function involving rock and fluid properties. The purpose of this study is to provide a method, based on steady-state equations, of estimating the direction and relative magnitude of permeabilities in an oil reservoir from field pressure data and well locations only. The method presented is based on work by Muskat6 which shows that Laplace&apos;s equation represents the steady-state pressure distribution for homogeneous fluid flow in homogeneous, anisotropic media if the co-ordinates of the system are shrunk or expanded by replacing x with it is desirable that data be obtained early in the history of a field because knowledge of an anisotropic condition would allow new wells to be spaced in such a manner that reservoir development and subsequent secondary recovery programs could be planned more efficiently. THEORETICAL CONSIDERATIONS A brief discussion of the theoretical basis on which the graphical solution was developed is presented in this section. Muskat&apos;s two-dimensional6 olution for the pressure distribution in an homogeneous, anisotropic medium with an homogeneous fluid flowing can be algebraically manipulated to show that the isobaric lines are perfect ellipses. The ratio of the major axis to the minor axis, a/b, is related to the permeability ratio, k,/k,, as follows. alb = dk,/k,--...........(1) It can also be shown that the pressure varies linearly with the logarithm of the radial distance from the producing well. However, the gradient along any ray is a function of the orientation of that ray, and a ..xiable is present when anisotropy exists which cancels out for a radial (isotropic) system. For a system such as that described, a dimensionless pressure-drop ratio was developed which is completely independent of the actual magnitude of the pressures. This was done by arranging Muskat&apos;s solution in such a way that aIl variables cancelled out except k,/k, and well positions. However, this solution depends on having a co-ordinate system with axes coinciding with the major and minor axes of the elliptical isobars. Thus, it was necessary to introduce a co-ordinate system rotation factor. The two unknown variables are then k,/k. and 0, and the two measured dimensionless pressure-drop ratios are related to the unknown variables as follows.

By E. Eichen, G. S. Ansell. L. R. Sefton

A Technique for the Preparation of Thin Films of Two-Phase Alloys Suitable for Use in Transmission Electron Microscopy In order to obtain foil sufficiently thin to permit transmission electron microscopy of two-phase alloys, particularly alloys in which the second phase is present as a very finely dispersed second phase, a technique has been developed to permit the thinning of these materials without either the large degree of pitting present in the electrochemical or chemical thinning process or the slicing of the second phase particles accompanying the mi-crotoming process. The metal or alloy to be thinned is first ground to initial sheet thickness of approximately 0.002 in. by hand grinding on 4/0 emery paper. This starting sheet of material is then reduced in cross section by an air-abrasion technique using an S. S. White dental abrasive unit. This unit consists of a supply of compressed CO, which provides a stream of high velocity gas impinging on the metal surface. Incorporated in the machine is a hopper-type of device in which fine abrasive particles of alumina are introduced into this high velocity gas stream. The abrasive particles are irregular in shape, approximately 30 across. If any particles are introduced into the sample during thinning, they should be readily observable. Impingement of this gas abrasive mixture on the metal surface causes rapid removal of the metal in a rather uniform manner. The rates of metal removal may be adjusted by both regulating the gas pressure and amount of abrasive material introduced into the gas stream. By moving the gas stream abrasive mixture slowly about the specimen or sheet surface, a large area of the sheet may be uniformly reduced to a thickness which is then suitable for use in transmission electron microscopy. Attendant with this metal removal is a result in cold working of the metal surface due to the impingement of the abrasive particles. The resultant foils, therefore, if made from materials which are desirable to view in the annealed condition, have to be subsequently heat treated. If the alloy from which these foils have been made has been initially heavily worked or deformed during manufacture, then no subsequent heat treatment is, necessary as in the case of the SAP-type alloys. Following this initial abrasive thinning technique, the material is then given a final electropolish which is just sufficient to remove any oxide which has formed on the metal surface during the abrasion technique. Care has to be exercised in this technique to make sure that none of the attendant problems associated with the chemical or electrochemical removal process are encountered. An electrolyte solution which has been found suitable for aluminum-aluminum oxide SAP materials is one containing 78 ml of perchloric acid, 120 ml of distilled water, 700 ml of ethanol, and 100 ml of butylcellosolve. The current density used is 1 amp per sq cm and a polishing time of 3 sec on each side of the foil is used. Extreme care must be used in choosing the current density and time to ensure that just the oxide film on the specimen is removed. Times or current density which are greater than this will lead to perforation of the film due to the removal of the A1,0, particles or a complete loss of the film due to complete solution of the matrix. Once the oxide film is removed the specimens must be kept in alcohol until placed in the microscope to prevent any further oxidation. Fig. 1 shows -an electron micrograph at X28,000 of a thin foil of an aluminum-aluminum oxide SAP-type alloy prepared using this technique. The alloy consists of a matrix of commercial purity aluminum containing a very finely dispersed second phase of aluminum oxide flakes. In the electron micrograph, the dark patches are the aluminum oxide particles. The lighter portions of the micrograph are the aluminum matrix. Within the aluminum matrix, the dislocation structure of the alloy is clearly visible. This structure consists of intersecting twin boundaries and single dislocations. No abrasive particles were observed in the samples. In addition, thin films of commercial purity aluminum were prepared using this method and observed in the electron microscope. Here also, there was no evidence of abrasive particles introduced in the samples. The technique presented provides a satisfactory method for the production of thin films of aluminum-aluminum oxide SAP-type alloys for use in transmission electron microscopy where none of the usual thinning techniques appears to be satisfactory.

Jan 1, 1962

By P. Greenfield, C. C. Smith, A. M. Taylor

J. E. Harris (Berkeley Nucclear Laboratories, England)—Greenfield et al.11 attribute abrupt changes in slope of their log o/log i curves for heat-treated Mg/0.5 pet Zr alloy (zA) to &apos;atmosphere&apos; locking. It is proposed here that a more reasonable explanation of the apparent strengthening at low rates of strain can be based on precipitation either during the preanneal or during the creep tests. All the tests were carried out above 0.5 Tm where solute atmospheres are likely to be largely evaporated2 and can migrate sufficiently rapidly so as not to impose any &apos;drag&apos; on the moving dislocations. McLean3 has derived an expression for determining the temperature Tc above which, due to the high-migration rate of the atmospheres, Cottrell or Suzuki locking can play no part in determining creep strength. This expression, which holds for an applied shear stress of not greater than 5 X 107 dynes per sq cm is: Tc/Tm= 7/6.8 - log10? where i = secondary creep rate The values for T, corresponding to the maximum and minimum reported creep rates at each temperature have been calculated from the data of Greenfield et al. These are given in Table VII. All the test temperatures were above T,, the margin being greater for the higher temperatures and for the lower strain rates where the breaks in the log s/log ? curves occurred. Dorn and his collaborators14, 17 have studied systematically the effect of solute hardening on the creep properties of an A1/3.2 at. pet Mg alloy. In the temperature range where strain aging occurred in tensile tests, abnormally high-activation energies for secondary creep were obtained but at temperatures above 0.43 Tm, solute alloying did not have any effect on the creep parameters. Moreover, there have been no reports of any strain aging phenomenon during elevated temperature tensile tests with ZA material.18 Instead of the observed strengthening being due to atmosphere locking, it is now proposed that precipitates play an important role in enhancing the creep strength of the material. There are two possibilities—precipitation of zirconium hydride during the high-temperature preanneal and/or precipitation of the hydride or a-zirconium during creep. On the basis of the former the results can be interpreted in terms of a critical stress being necessary to force the dislocations through or over preexisting precipitates. From the latter, if the strengthening is due to pre- cipitation during the test then hardening should be associated with a critical strain rate. At low rates of strain, time is available during the tests for precipitation to occur either directly onto dislocations (thus pinning them) or generally throughout the matrix (which would impede dislocation movements). Examination of the data of Greenfield et al. suggests that both mechanisms may be operative since they observed precipitation during creep and also found that their alloys exhibited high-creep strength in the early stages of the low-stress tests, i.e., before creep-induced precipitation had time to occur. It is not easy to understand why they considered that precipitation of zirconium hydride is unlikely to occur at 600°C while it can take place in tests in air at as low a temperature as 200°C. Precipitation of the hydride during the preanneal cannot be ruled out merely on the basis of metallographic examination. Hydride precipitates in ZA type alloys are very small and can only be accurately resolved in the electron microscope.9 For example, in this laboratory20 hydride platelets with major dimensions <(1/10) µ have been observed by electron transmission through thin film specimens of hy-drogenated ZA material. Complex interactions between dislocations and such particles are illustrated in Fig. 12. Additional evidence for precipitation during pre-annealing is provided by the data presented in Greenfield&apos;s Fig. 1 and Table IT. These show that the creep strength at 200o and 400°C increases with the time of preanneal at 600°C. Such increases cannot be explained on the basis of increases in grain size alone for further improvements in strength were observed when the material was annealed for longer times than that required to stabilize the grains. Although the main discussion is confined to ZA material, similar arguments can be used against the strain aging hypothesis proposed to explain the binary Mg/Mn alloy data. In this case no precipitation is possible during the preanneal, but precipitation-hardening during creep can occur.

Jan 1, 1962