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By P. S. Kotval, H. Hahell

PRECIPITATION of M23C6 carbides at grain boundaries in austenitic steels and nickel base superalloys has received considerable attention. Hatwell and Berghezan,1 in a study using carbon extraction replicas, observed that dendritic growth of the M23C6 carbide phase occurred at grain boundaries in austenitic steels. Merrick and Nicholson2 have observed that in thin foils of "Nimonic 75" alloy the precipitation of M23C6 carbide was discontinuous at grain boundaries. Lewis and Hattersley3 have suggested that the type of M23C6 precipitation observed in Ni-Cr austenites represented the early stages of discontinuous precipitation. In a more recent study, Singhal and Martin4 have concluded that grain boundary M23C6 precipitation involves the migration of an austenite grain boundary by a mechanism very similar to that proposed by Tu and Turnbull.5 Tu and Turnbull's suggestion essentially involves grain boundary migration under the driving force arising from the difference between the surface free energies of the opposite sides of the plate. Thus, Singhal and Martin's observation4 implies that the first stage of discontinuous precipitation has taken place and that the grain boundary has provided a diffusion short circuit for the sub-stitutional solute atoms (principally chromium) which assist the preferential growth of the M23C6 plate in contact with the grain boundary. However, no evidence of the characteristic cellular morphology typical of discontinuous precipitation was found in Singhal and Martin's studies. Presumably, this is due to the low volume fraction (i.e., low supersaturation of solute) of the precipitating carbide reported by Singhal and Martin.4 Recently, Raymond6 has studied precipitation of the M23C6 carbide in Incoloy alloy 825 and shown that the growth of this phase is perpendicular to grain boundaries at 1400°F and in the plane of the grain boundary at 1700°F. The former aging condition resulting in discontinuous or "cellular" precipitation. Raymond has suggested an explanation for this behavior based on the relative rates of chromium diffusion by volume and grain boundary diffusion at the two different aging temperatures. In the course of a recent investigation on precipitation behavior in several ' strengthened superalloys, precipitation of M23C6 carbide at grain boundaries was studied. Under conditions of a high degree of supersaturation, the M23C6 carbide precipitates in the discontinuous or cellular morphology in Waspalloy (Ni-18.51 Cr-2.0 Fe-3.53 Mo-1.16 Al-2.78 Ti-0.09 C). This note presents electron microscopy observations of this mode of precipitation and its effect on mechanical properties. Specimens of Waspalloy after "solution" heat treatment at 1950°F show essentially single phase matrix with a few residual particles of "primary" MC carbide. In normal commercial heat treatments, precipitation of Ni3(Al,Ti) ordered fcc r' phase occurs throughout the matrix and M23C6 precipitates as globular particles at the grain boundaries. In these commercial heat treatments the degree of supersaturation during precipitation is low. However, if specimens of Waspalloy are quenched from the solution heat treatment temperature of 1950°F and then aged at an aging temperature where the degree of supersaturation is high, discontinuous precipitation of M23C6 occurs. Figs. 1 and 2 show thin foil micrographs of Waspalloy, solution heat treated at 1950°F, water quenched, and aged at 1292° and 1598°F, respectively, for 500 Fig. 1—Thin foil of Waspalloy, solution heat treated at 1950°F for 1 hr, water quenched, and aged for 500 hr at 1292°F. Magnification 15,500 times. Fig. 2—Thin foil of Waspalloy, solution heat treated at 1950°F for 1 hr, water quenched, and aged for 114 hr at 1598° F. Magnification 13,000 times.

Jan 1, 1970

By T. G. Lovering

Nonparametric statistical tests have practical application to many geological problems because, unlike the standard statistical tests, they do not require assumptions regarding the form of the population frequency distribution. Many of them do not even require that the variable be susceptible to numerical measurement. These tests are useful either 1) for geological data representing population distributions of unknown form, or otherwise not meeting the requirements for standard parametric tests; or 2) for sample attributes that cannot be measured but only ranked in order of relative magnitude. The application of two such tests will be illustrated. The Kolmogorov-Smimov test will be used to test for significant differences in copper distribution in samples of two rock types; the Spearman rank-correlation method will be used to determine whether there is a significant association between intensity of rock alteration and copper content of the rock. Nonparametric tests are, in general, quicker and easier to perform than the corresponding parametric tests, and they may be applied to a greater variety of data. They are not as powerful as the standard tests if used on data to which the latter are applicable, and computer programs utilizing them are not generally available. The use of standard or parametric statistical procedures for the interpretation of measured geological data is familiar to most mining engineers and explora- tion geologists. The computation of product moment correlation coefficients on sample assays for more-than one component is already standard procedure in some company operations, as is the use of Student's F test and Snedecor's F test for the comparison of means and variances of sample groups. The application of these three tests is limited by the prerequisites that the samples must be random, independent representatives of normally distributed populations and that the variables involved must be measurable. If such tests are applied to data which fall short of fulfilling these prerequisites, then the probability level attributed to the computed statistic is invalid and the conclusions based thereon may be erroneous. A number of nonparametric, or distribution free, statistical tests have been developed for use with data which are not amenable to standard parametric procedures. These tests have been widely used in the behavioral sciences such as psychology and sociology for some time, but their application to geologic problems is relatively new. Nonparametric tests may be grouped into two main categories: those which test for significant differences in a single variable by comparing either sample values with a standard value or representative values between two or more groups of samples; and those which test for significant association between pairs of variables in a single group of samples. The versatile chi square test, the Kolmogorov-Smirnov one and two sample tests, the Wilcox matched pairs signed ranks test, the median test, the Mann-Whitney U test and the Cochran Q test are examples of nonparametric tests with demonstrated or potential geological applications that belong in the first category. The contingency coefficient, Spearman rank correlation coefficient, Kendall rank correlation coefficient and the

Jan 1, 1963

By G. K. Manning, W. E. Few

T has been known for some time that both'inter-granular carbide and intergranular oxide phases cause brittleness in molybdenum. Parke and Ham' indicated that 0.0025 pct 0 present in molybdenum after solidification from the melt was sufficient to induce intergranular brittleness during forging. However, material containing 0.06 pct C could still be forged. However, adding this amount of carbon to insure deoxidation causes the formation of carbides on freezing. These carbides are precipitated at grain boundaries, and Rengstorff and Fischer' have shown they have an unfavorable effect on the room-temperature ductility of molybdenum. Take? in 1928 proposed that the solubility of carbon was a constant value of 0.30 pct from room temperature up to 1800°C. In 1935, Sykes, Van Horn, and Tucker' obtained X-ray data suggesting that the solid solubility of carbon in molybdenum was between 0.07 and 0.09 pct at temperatures from 1500" to 2100°C. The a-solubility line for carbon was included in the Mo-C diagram given in the Metals Handbook as a tentative line based on the data of Sykes, Van Horn, and Tucker. In order to determine the partial phase diagrams for these systems, it was necessary to construct a high-temperature furnace suitable for heat treating molybdenum at temperatures up to 4000°F. A molybdenum resistance furnace was built for this purpose in which samples could be heat treated in a purified atmosphere and quenched from any desired temperature.' Experimental Work Solubility of Carbon: Arc-cast molybdenum supplied by the Climax Molybdenum Co. and 18-gage molybdenum wire samples produced by powder metallurgy at the Fansteel Metallurgical Co. were used in determining the a-solubility line for the MO-C system. The cast molybdenum contained 0.032 pct C initially. Two lots of 18-gage wire were used, one containing 0.011 pct C and the other 0.005 pct C initially. All material contained a carbide phase as received. Fig. 1 illustrates the carbides found in the untreated material. Heat treatment in a purified hydrogen atmosphere was found to reduce the carbon content in the as-cast molybdenum. Purified argonT also decarburized molybdenum samples at temperatures above 3500°F; however, the carbon content remained constant during heat treatment in purified argon at lower tem- peratures. The argon was purified by passing it over titanium at 750 °C and then through a magnesium perchlorate drying tower. The hydrogen was purified by passing it through a commercial hydrogen deoxidizer, followed by a drying tower. Specimens having different initial carbon contents were heat treated in argon at 3500°F for periods ranging from 5 min to 5 hr and were analyzed for carbon. Samples of the same final carbon content had the same microstructures regardless of time at temperature. Furthermore, a gradient between center and surface in the amount of undissolved carbide particles present was never observed. It was concluded that at these low carbon levels, and at the high temperatures involved, diffusion proceeds so rapidly that the specimen is always substantially homogeneous in carbon content, in spite of the gradual loss in carbon. Based on the above findings, the following procedure was used to determine the carbon-solubility limit at 3000°, 3500°, and 4000°F. At each of these temperatures, a number of samples were heat treated, as shown in Table I, and rapidly cooled to room temperature. Since the samples lost carbon in proportion to the length of time heated, a series of samples were obtained of varying carbon contents. By use of a rapid cooling rate, the phases present at the high temperature were retained at room temperature. All samples were examined microscopically. Those found to contain either no excess carbide phase or only a very small amount were then analyzed for carbon. The samples actually analyzed for carbon

Jan 1, 1953

By G. R. Gardner, D. H. Davis

INCREASING realization of the importance of dust control, and the recommendations of various agencies, have led the mining industry to become actively concerned with this problem. The background and necessity for adequate dust-suppression measures have been discussed in a number of publications, including those of the U. S. Bureau of Mines, and the use of spray water to reduce dust at the face and on roadways has been recommended. The problem resolves itself into obtaining adequate dust reduction at a reasonable cost. Inasmuch as the term "adequate dust suppression" has never been clearly defined, nor have permissible limits of dustiness (in terms of dust count) been established, it is apparent that any method selected may be required to meet additional demands. Until the industry has been given some indication of permissible limits of dustiness, no permanent solution is possible. Progress will be somewhat handicapped until such information is available. In addition, dust reduction must be obtained without the addition of any excessive moisture to the coal, since consideration must often be given to: I. Quality standards, particularly reduction in heat value. 2. Handling characteristics, particularly in regard to unloading from railroad cars and bins. 3. Application of dry methods of coal cleaning. 4. Necessity for fine screening within specified limits of oversize and undersize. Little detailed information is available as to the advantages and disadvantages of the several methods of water distribution, the location and protection of sprays, operating data on pressure, quantity of water, and so forth, and results obtained. In 1940 an investigation was undertaken to determine and evaluate the principal factors involved. This paper constitutes a progress report on this work and cannot in any way be regarded as complete on any one of the several phases. CLASSIFICATION OF DUST SOURCES The various sources of underground dust may be classified as primary or secondary. A primary source is one associated with appreciable degradation of size, that is, where the greater part of the actual fines capable of becoming air-borne dust are produced. A secondary source may be considered as one in which the greater part of the fines have been produced at some previous operation and are in such condition that they can be dispersed as air-borne dust. These conceptions appear to be of practical significance, as experience indicates that when dust is controlled at the primary sources the importance of secondary sources is minimized. For these reasons, investigations to date have been concerned principally with the primary sources of dust, and this paper is concerned particularly with one of these-namely, undercutting. In accord with the foregoing definitions, the sources to which the following opera-

Jan 1, 1942

By F. O. Garrabrant

POWER is furnished to the Climax Molybdenum Co. by the Public Service Co. of Colorado over two 100,000-volt line to a bank of three 3333-kva. Transformers 100/13.8 kv. These transformers arc so designed that with the addition of forced cooling their capacity may be increased 33 1/3 per cent at 12,000-ft. altitude. Under present conditions, these transformers are operated at 140 per cent of their rating with forced air cooling. On the secondary side of this bank there is a 15-kv., 1200- amp. Westinghouse oil circuit breaker provided with automatic reclosing relays allowing three successive short circuits before lockout. From this breaker 13.8-kv. power is transmitted to a central switching station (Fig. I) where all circuits radiate to the different operations of the property. Each circuit is protected by a 23-kv., 600-amp. oil circuit breaker with by-pass and isolating disconnecting switches. MINE Power at 13.8 kv. enters the mine through a ventilation raise over a three-conductor, size 1-0 varnished cambric insulated, leaded, steel-wire armored cable, insulated from 17 kv. This power is received and distributed through one switching station and four underground substations, shown in Fig. 2. No. 370 substation (Fig. 3) contains three 250-kva, 13,800/440-volt, single-phase Pyranol transformers protected on the high-voltage side by a 600-amp. manually operated oil circuit breaker. This station serves 20 slusher-hoist motors, a 45-kw., three-phase, 220-volt electric furnace, a Massco hot miller for tempering and milling Timken detachable bits and a hoist with 175-hp. motor on the No. 3 development shaft. Also at this shaft are three pumps. One two-stage pump, 1200 gal, per min., 100-ft. head, 3600 r.p.m., driven by a 150-hp. motor, is at the bottom of the shaft. Two deep-well pumps, 500 gal. per min., 500-ft. head, are at the collar of the shaft. Under normal operation the one pumping 1200 gal. per min. is controlled by a float switch to take care of the water. If this pump fails, or if its capacity is insufficient, the first 500-gal. pump is automatically started, and if still more capacity is needed the second 500-gal. pump automatically starts. Time delay relays are provided on the deep-well pumps, so that if power fails the column will have time to drain before the pumps restart. On failure of any of these, an alarm is sounded in the train dispatcher's office, so that mechanics can be sent to ascertain the cause of failure and make repairs. The cable from No. 370 substation is run to the switching station, in which are four15-kv., 600-amp. direct-current solenoid-operated oil circuit breakers. The current for operating and tripping is furnished by a 125-volt storage battery. All breakers are operated from the switchboard in the compressor room. One circuit from this switching station goes to the

Jan 1, 1944

By J. D. Rice, P. L. Wearden, W. L. Hensou

Solutions to the unsteady-state partial water-drive reservoir performance problem can be obtained through the use of analogue computers or high-speed electronic digital computers. The solutions that have previously been resolved for use on digital computers, however, demand a knowledge of the aquifer parameters. Generally, the analogue computers now in use do not require this knowledge. A solution is presented herein where the aquifer performance, expressed in terms of difference equations, is related to the reservoir performance as expressed by the modified Scbiltbuis material-balance equation. A numerical procedure for a medium-sized digital computer also is presented in which a solution to the set of equations defining the aquifer and reservoir performance is obtained and the aquifer parameters (permeability and sand thickness) are automatically optimized while simultaneously matching the known pressure behavior. Predicted pressure behavior can be calculated using rates from any assumed future production practice. The procedure provides an output format which presents the cumulative, incremental and average rate of natural water influx, the per cent gas-cap expansion, the calculated reservoir pressure, the measured reservoir pressure, and the difference between the measured and calculated pressures. Results of a test problem are presented in comparison with results obtained by the Bruce Analyzer, Ohio Oil Co. 's Pace General Purpose Analogue Computer, and Sun Oil Co.'s Single-Pool Electronic Reservoir Analyzer. These results indicate that unsteady-state reservoir perlormance for a single-pool system can be adequately simulated by a numerical method employing a digital computer and that the special-purpose analogue computer can be supplanted by this method. INTRODUCTION The numerical approach to the unsteady-state partial water-drive reservoir performance problem heretofore has been limited in that solutions have been resolved only for certain fixed parameters. Also, prior to the advent of high-speed electronic digital computers in the last few years, calculations were so tedious and time-consuming that they ordinarily were neglected, or some other means of obtaining the solutions were used. The analogue approach had been used for obtaining solutions to the transmission-of-heat problem and, consequently, means were developed for applying the electrical analogue to the unsteady-state reservoir performance problem. Bruce submitted a paper for AIME publication in Sept. 1942, in which he described an electronic device (now called the Bruce Analyzer) for analyzing the water-drive performance of any reservoir, based on either steady or unsteady-state flow characteristics. 1 Sun Oil Co. adopted the analogue approach in 1949 and now has two special-purpose high-speed electronic reservoir analyzers in use.2,3 Two main features of Sun's analyzers are (1) the high repetitive rate of reproducing the entire history of reservoir performance cyclically a number of times per second, and (2) the elimination of the necessity of knowing the properties of the associated aquifer. Since the advent of larger and faster digital computers, the possibility of incorporating this second feature into a numerical approach appeared feasible. Previous work has been done and material published covering the application of numerical methods to the behavior of the pressure with respect to time at any point in an associated aquifer? However, the aquifer parameters must be known from some source. The material presented in Ref. 4 has been used to a great degree in developing the numerical method described herein. DIFFERENTIAL EQUATION AND BOUNDARY CONDITIONS The problem of simulating the performance of a reservoir and the associated aquifer is to determine the characteristics of the aquifer such that the

By P. E. Arnold, G. S. Ansell

RELAXATION in metals has been studied in detail by many workers in recent years.1-5 These studies have shown that there is an energy-loss peak observed in a metal placed in mechanical resonance at low frequencies which may be correlated with various metallurgical processes. These experiments have been largely used to study single-phase materials. In order to study the effect of a finely dispersed second phase in a metal matrix upon this phenomenon, the relaxation behavior of an aluminum-aluminum oxide SAP-Type alloy in both the fine-grained as-extruded and coarse-grained recrystallized conditions was investigated by the use of internal-friction measurements. The alloys studied, designated MD 2100, consist of a matrix of commercial-purity aluminum containing a finely dispersed second phase of aluminum oxide. The aluminum oxide is present in this alloy in the form of fine platelets approximately 130A units thick and several microns on edge. The mean free path betwen dispersed platelets is approximately 0.5 p. The grain size of this alloy is extremely stable at temperatures as high as the melting temperature of the aluminum matrix. In the as-extruded condition the grain diameter is several microns, while in the recrystallized condition it is several millimeters in diameter. The damping characteristics of the alloy samples were determined using a torsional-pendulum device. The internal-friction constant was determined for this alloy in both the fine-grained as-extruded and coarse-grained recrystallized conditions over the temperature range from 343" to 923°K at frequencies of 0.9, 1.3, and 1.8 cycles per sec. An internal-friction peak was observed in testing the fine-grained alloys which was not observed for the coarse-grained alloys. This peak, which might be associated with a type of grain-boundary relaxation, was observed at each of the three different test frequencies for the fine-grained sample. The temperature at which the relaxation peak occurred for each of the three different frequencies is shown in Table I. From these data an activation energy of relaxation for each pair of frequencies was determined by comparing the temperature shift of the relaxation peak with frequency between each of the test frequencies, assuming that an Arrhenius-type rate equation is applicable. The activation energy of relaxation determined from these data is also shown in Table I. The mean value of the activation energy was about 6 kcal per mole. The activation energy for the relaxation process determined in this investigation indicates that the relaxation associated with the grain boundaries in this aluminum-aluminum oxide SAP-Type alloy is quite a different process than grain boundary relaxation in single-phase aluminum alloys. In these latter alloys, the activation energy for relaxation has been found to be the activation energy for self-diffusion, approximately 36 kcal per mole1,2 Where the activation energy is the same as the activation energy for self diffusion, it has been proposed that the relaxation phenomena is dependent upon vacancy formation and motion. It is apparent therefore, that, in this aluminum-aluminum oxide SAP-Type alloy, the relaxation must be due to another type of atom transport. It has been shown previously in studies of the high-temperature, low-stress, steady-state creep behavior of as-extruded aluminum SAP-Type alloys, that the activation energy for steady-state creep is one that may be characterized by the nucleation of dislocations from the grain boundaries. It is proposed that the relaxation behavior observed here is due to a similar effect. In this case, the internal-friction peak is a resonance behavior due to the time-dependent nucleation of dislocations from grain boundaries in the sample. A process of this type would have an activation energy which is undoubtedly stress-dependent and of the form Q = Q, + (dQ/du)u

Jan 1, 1962

Discussion of the paper of HOWARD N. EAVENSON, presented at the New York meeting, February, 1915, and printed in Bulletin No. 98, February, 1915, pp. 413 to 430. WILLIAM H. GRADY, Bluefield, W. Va.-Mr. Eavenson gave a comparison between accidents in the State of West Virginia and in the Pocahontas field. The figures quoted are, I presume, taken from the reports of the State Mine Inspector. There are no statistics available, in readily accessible form, giving a comparison between the Pocahontas field and the mines of the United States Coal & Coke Co. which are a part of the field. It occurs to me that the paper would be more complete with these data and I will say that the mines of the Pocahontas field produced during the year 1913 about 15,000,000 tons, about 3,000,000 tons of which was produced by the United States Coal &Coke Co. This gives an indication of the extent of its operations. The Pocahontas field lies largely in the counties of McDowell, Mercer, and Wyoming in West Virginia, and Tazewell in Virginia.: Without consulting maps, I should say that all of the acreage under operation at present by this company lies wholly in McDowell County and that the average conditions off roof top and bottom in its mines are the average of the county, but that the worst conditions in some of these mines are the worst to be found in the county. The average conditions in Tazewell County are about the same as in McDowell County, except that the average thickness of the seam is much greater. The average conditions of top and roof and bottom are better in Mercer and Wyoming counties than in the mines of the United States Coal &. Coke Co.; the worst conditions in these counties are not so bad as in McDowell and Tazewell counties and the best are better than those encountered in McDowell and Tazewell counties; also the thickness of seam is less in Mercer and Wyoming counties. THOMAS W. DAWSON, Scottdale, Pa. (communication to the Secretary*).-The H. C. Frick Coke Co., the mines of which are in Fayette and Westmoreland counties, Pennsylvania, in the Connellsville coke region, has been pursuing a safety campaign for a number of years and a short resume .of its practices will be of interest in connection with Mr. Eavenson's paper.

Jan 5, 1915

By G. B. Gould, H. L. Brunjes

The softening temperature of coal ash, as determined in the laboratory, has been used for years as an indication of the tendency of coal to form clinker and slag. It has not, however, provided an index of unfailing and complete reliability for forecasting the relative performance of different coals, even in the same plant and under the same conditions of operation. A large amount of investigation has been done in attempts to account for this, but practically all of this has been in the direction of studying the chemical constitution of coal ash. Much has been learned, but without much progress toward a better practical application of knowledge to the selection of coal. There has always seemed to be an important factor that eluded discovery. It has long been recognized that the ash-softening temperature as determined in the laboratory had one weakness, in that it represented the temperature at which a thorough mixture of the whole ash of the coal would melt, the mixing having taken place before the heal was applied. This does not, of course, simulate what takes place in practice. With certain exceptions, which will be noted later, almost all of the investigations that have been made, especially the chemical studies of coal ash, have likewise dealt with a mixture of the whole ash in the coal. The present investigation differs from these fundamentally in its approach to the problem. It started from the observation that some clinkering and slagging obviously takes place in a boiler furnace at temperatures below the laboratory-determined ash-softening temperature of the coal. Knowing that coal as it is shipped to market is a heterogeneous mixture of diverse mineral substances, each of which may act independently of the others in the initial stages of clinker and slag formation, it seemed logical to investigate separately the softening temperature of the ash in physically separable portions of the coal, and to determine the relative quantities of ash contributed by each portion. While the data are far from complete, covering as they do only a few coals, and while the conclusions to be reached from the data at this stage arc, in some measure, speculative, they are presented at this time because

Jan 1, 1940

By F. C. Sturges

[CONTENTS PAGE ................. Introduction-Grouting in Mines. By F. C. STURGES. I Use and Technique of Pressure Grouting in the Construction Industry. By V. L. MINEAR . 3 Technique of Pressure Cementing in the Petroleum, Mining, and Construction Industries. By WY. D. OWSLEY and R. E. MOELLER. ..................... 9 An Example of Controlled Pre-grouting in Shaft Sinking. By R. H. ALLEN and J. W. GALPIN. 15 ........ Solidifying Mines and Shafts Areas by Pressure Grouting. By B. H. MOTT 17 .............. Grouting in Southeast Missouri District. By W. W. WEIGEL 20] Introduction-Grouting in Mines By definition the word "grout" means a thin mortar, or a kind of plaster or cement, and "grouting" means to fill up or finish with grout. The words "cement," "plaster" and "mortar" mean a substance that is used in a soft state which subsequently hardens. Thus, grouting is the filling of void space with a substance that hardens. Construction cements are the most common substances used, either by themselves or in mixtures, but the term grouting is applied quite correctly when other substances such as plastics and certain chemicals are used. Also, the use of the term grouting to cover the filling of voids with materials that do not actually become hard, such as the flotation tailings used in grouting in the southeast Missouri lead district, should be considered correct, as some stiffening does take place and, anyway, it is a better descriptive term than any substitute. Engineers are interested in grouting because some of the materials with which they must work contain voids, and certain conditions can be improved if these voids can be filled with something solid and permanent. Grouting is done to accomplish several purposes: I. To stop the passage of fluids and gases, 2. To cement materials together to make them stronger, and 3. To prevent consolidation of materials by filling void space with something solid as a replacement for the air and water that could be forced out under load. The construction industry uses grouting extensively for all three purposes. Grouting is used to stop water percolation under and around dams. It is used to control water flow in tunnel driving and in shaft sinking. It is used to improve foundation conditions under civil engineering structures by permanently filling void space and thereby reducing settlement, or by cementing broken rock together and increasing its supporting strength. The oil and gas industry does a lot of grouting, primarily to stop the passage of gases and fluids. The search for oil at increasingly greater depths has meant greater investment per well, and the oil industry has spent large sums on development of improved drilling methods. This

Jan 1, 1947

By D. A. Stevenson, R. A. Burmeister

Single-phase silver antimony telluride has been prepared by zone-melting techniques using initial compositions of A new phase appears upon prolonged annealing of this material, but the reaction does not appear to be a simple eutectoid decomposition. A complete analysis of the phase equilibria is complicated by the slow kinetics involved. The Hall coefficient, magneto -resistance, electrical resistivity, and Seebeck coefficient are all sensitive to the presence of second phases. The low Hall mobilities measured for single-phase material indicate that the usual band theory is inadequate to explain the observed transport properties in the system. Density anomalies of up to 2.5 pet between measured and theoretical density were observed but are not conclusive evidence for a defect structure. COMPOSITIONS in the Ag-Sb-Te system have been studied previously by several investigators.1"18 The interest in this system arises from potential thermoelectric applications of alloys on the Ag2Te-Sb2Tes vertical section. Although the composition corresponding to the formula AgSbTe, has received most attention, it has been found to consist of more than one phase.7'8 A thorough understanding of the properties of this heterogeneous material has been impeded by both lack of knowledge of the properties of the homogeneous phases comprising it and the problem of analysis of transport properties in an inhomogeneous system. The present work describes the preparation of the homogeneous ternary phase and the corresponding electrical properties of both homogeneous and heterogeneous material. MATERIAL PREPARATION Most specimens for this investigation were prepared by encapsulating the elements in evacuated quartz tubes after which they were melted and homogenized in the liquid state. The ambient temperature was then dropped to 500°C and the resulting ingot zone melted. The growth rate, width of zone, stoichiometry, and number of passes have an effect on the resultant microstructure. Grains several centimeters in length were easily produced by this method. Other solidification techniques were also used, including uniform slow cooling of the entire specimen and rapid freezing. The microstructures of specimens produced by these techniques frequently differed appreciably from similar compositions prepared by zoning. A variety of nonequilibrium microstructures characterized by long needlelike particles resulted from the rapid-freeze method. PHASE EQUILIBRIA The lack of information on phase equilibria is a major difficulty associated with a comprehensive study of the Ag-Sb-Te system. Considerable confusion has resulted from the use of the formula AgSbTe, to identify the cubic ternary intermediate phase even though it has been established that material of this stoichiometry normally contains AgzTe as a second phase.798 In this paper, silver antimony telluride will denote the cubic ternary intermediate phase comprising the major portion of AgSbTe,. The term "single phase" will denote material which consists of only the cubic phase (as evidenced by metallographic examination and X-ray diffraction) and the term heterogeneous will describe multiphase material containing AgzTe, SbzTe3, or other phases in addition to the cubic phase. The single-phase material may actually contain a variety of inhomogeneities—gradual changes in composition on a macroscopic scale, localized fluctuations in composition, clusters or other products of early stages of the precipitation process, and a variety of point and line defects—all of which will not be detected by the present techniques for determining homogeneity. Single-phase material has been prepared from compositions close to 59 mole pct SbzTe3 21 (this notation refers to the location on the Ag,Te-Sb2TeS vertical section). Zone widths of =2 cm and growth rates 51.2 cm per hr were used. The single-phase region at elevated temperatures extends off the vertical section to a composition which can be expressed approximately as Ag,,SbzgTes,.9 The latter two compositions as well as AgSbTe, are represented in the conventional Gibbs triangle in Fig. 1. It is not presently possible to ascribe exact values to the limits of the single-phase region on a given isotherm or vertical section due to the extremely

Jan 1, 1964

By C. T. Liu, J. Gurland

The deformation behavior in tension of spheroidized carbon steels was studied at room temperature as a function of carbon content, 0.065 to 1.46 wt Pct, and carbide particle size, 0.88 to 2.77 p. It was found that the Hall-Petch strength-grain size relation is directly applicable to the yield and flow stresses of the two lower-carbon steels , 0.065 and 0.30 pct C. The strength data for the medium- and high-carbon steels, 0.55 to 1.46 pct C, also satisfied the Hall-Petch relation, provided that these data are based upon the particle spacing. Beyond 4 pct strain, the flow stress data of all the steels studied could be represented by the same Hall-Petch relation with dinerent spacings for grain boundary and particle strengthening. The behavior of the higher-carbon steels was consistent with the postulated formation of a dislocation cell network during processing and initial deformation (up to 4 pct strain). The cell size was assumed to be equal to the planar particle spacing. The true stress at the ultimate tensile strength was also found to be a function of the particle spacing. At a given temperature and strain rate, the yield and flow stresses of carbon steels depend on the type and dimensions of the microstructure. Starting with the work of Gensamer et al. in 1942,' experimental studies on pearlitic and spheroidized carbon steels revealed that the strength of steels is a function of two main parameters: the ferrite grain size2'3 and the carbide particle spacing;1'4'5 on this basis, two different strengthening mechanisms have been developed to apply to steels of low and high carbon contents, respectively. In polycrystalline iron and mild steels the grain boundaries are regarded as the major structural barriers to slip. The relation between strength and grain size is generally represented by the Hall-Petch equation which is based on a linear proportionality between strength and the inverse square root of the average grain size.2'3y677 However, Gensamer et al.' and Roberts et related the yield strength of medium -and high-carbon steels to the carbide particle spacing alone, and they found a linear relation between the logarithm of the mean free path in the ferrite and the yield strength in both spheroidized and pearlitic steels. By means of the electron microscope, Turkalo and LOW' extended the study to finer structures; they concluded that the logarithmic relation is not valid for the entire range of microstructures unless grain boundaries are also included in the measurement of the mean free path. For the specific case of spheroidized steels, Ansell and aenel' found that the yield strength data,4'5 when plotted as a function of mean free path, fit the Hall-Petch equation; however, T'ysong found that the same data fit the 0rowanl0 relation if a planar inter-particle spacing is used. Recently Kossowsky and ~rown" studied the strength of prestrained spheroidized steels, 0.48 and 0.95 pct C, and concluded that the strength due to the carbide dispersions varies linearly with the reciprocal of the square root of the mean free path between carbide particles and dislocation networks. Such networks were first observed by Turkalo." The conclusion common to all these studies is that the available slip distance in the ferrite is the most important variable in determining strendh. Previous work on carbon steels is restricted to limited composition and strain ranges. The mechanism which governs the flow properties is not clearly understood, and, in particular, little is known about the composition dependence of the transition between grain boundary strengthening and particle hardening. The purpose of the present work is to investigate the strengthening mechanism in spheroidized steels over a wide range of carbon content, 0.065 to 1.46 wt pct, and plastic strain, yielding to necking. The spheroidized structure was chosen because of its relative simplicity and the relative ease of control and measurement of the structural parameters. The experimental work is limited to tensile testing at room temperature at constant extension rate. The effects of the carbide particles on the fracture behavior of spheroidized steels are discussed elsewhere.13 EXPERIMENTAL PROCEDURE Eight different grades of vacuum-cast carbon steels were supplied in the form of forged and rolled plate by the Applied Research Laboratory of the U.S. Steel Corp. The compositions furnished with these steels are given in Table I; the carbon content ranges from 0.065 to 1.46 wt pct, or from 1.0 to 22.3 vol pct of carbide. The steel plates were cut transversely into rods a little larger than the test specimens, 1 in. gage length, i in. diam. The rods were austenitized in air (enriched with CO by a consumable carbon-rich muffle) at 50° C above theA, orA., temperature for 2 hr and then quenched in oil with vigorous stirring. The as-quenched rods were tempered in two stages in order to obtain the desired distributions and sizes of carbide particles. The rods were first tempered at 460° C for 10 hr and then at 700" C for periods ranging from 4 hr to 3 days, in vacuum. After final machining, all specimens were vacuum-annealed again at 650°C for 1 hr in order to relieve residual stresses. The tension tests were carried out in two steps. The initial part of the load-strain curve, up to about 2 pct strain, was determined on a Riehle testing machine with an extensometer of small strain range, 4 pct strain, in order to obtain the yield and initial flow piopertiesi As soon as the first part of the test was finished, the specimen was placed in an Instron testing machine equipped with a strain gage extensometer with a maximum strain range of 50 pct. The load-strain curve to fracture was

Jan 1, 1969

By H. A. Wahl, J. M. Campbell

This study extends our information on solid-liquid slurries to the flow of sand in horizontal fractures. Inasmuch as this is basically an unsteady-state process, a comprehensive photographic study was undertaken in a 10-ft windowed cell to determine if the basic flow regimes described for steady-state flow in pipes applied to the subject process. Since the number of potential variables far exceeds the capacity of a single study, emphasis has been placed on the effects of sand concentration, oil viscosity and oil flow rate. The extensive photographic evidence obtained has proven very valuable in gaining an insight into the basic flow mechanisms. Being able to follow visually the flow characteristics that accompany the quantitative data is valuable in the application of the results. Although the use of dimensionless parameters was carefully investigated. it was found that the data obtained could be more easily, and as accurately, correlated by judicious use of the dimensional variables investigated. However, a study into the feasibility of scaling slurry flow was made in the event this technique is justified in future investigations. The data presented show that the pressure behavior observed in solids transport in pipes basically applies to slurry flow in horizontal fractures. The roles of the parameters are altered but a basic equivalence exists. The most significant correlating parameter was the oil viscosity (µo) and the bulk velocity of the slurry (vn), expressed as ''µv" product. The most significant correlation expresses the rate of advance of the sand as a function of the variables investigated. There are many practical ramifications of this phase of the investigation that should aid in better treatment design. Evaluation of sand advance rates provides a means of estimating sand placement efficiencies during a treatment and the resulting sand distribution in the fracture. The results show that sand placement efficiencies are low under typical treatment conditions. A brief description of the effects of overflushing is also included. INTRODUCTION The flow of sand-oil slurries in fractures is an area in which little basic knowledge is available. This stems to some degree from the fact that it is impossible to duplicate fractures at the surface. They occur in various shapes and sizes with an infinite combination of irregularities. Unfortunately, we can never "see" these fractures except in cores and by indirect means of measurement. In spite of this inherent difficulty, it is desirable to develop some basic concepts that will provide a better understanding of the sand transport mechanism. An insight into the problem is provided by investigations of fluid flow in rectangular conduits. Several studies on the flow of liquids in non-circular conduits1,13 show that a Reynolds number-Fanning friction factor relationship can be written if the hydraulic diameter is substituted for the regular diameter in a circular pipe. This hydraulic, or equivalent, diameter is taken as four times the cross-sectional area occupied by the flowing fluid divided by the wetted perimeter. Eq. 1 expresses an extension of this same work when applied to infinite parallel planes b distance apart.' Eq. 1 is a theoretical equation expressing the friction factor as a function of the Reynolds number for laminar single-phase fluid flow. This expression has been verified experimentally. The equivalent expression for a smooth circular conduit differs only in that the value of the constant is 16 instead of 24. Numerous studies have related friction losses to Reynolds number in both circular and non-circular conduits. These results are widely used and are not reviewed here. Huitt' investigated the effect of surface roughness on fluid flow in simulated fractures. He concluded that fluid flow in fractures may be treated similarly to fluid flow in circular conduits. This work, together with that of Nikuradse,' shows that surface roughness has no appreciative effect upon the resistance to flow in the viscous flow region. In the region of turbulent flow, surface roughness is a prominent factor. Hydraulic conveyance literature is another important source of information. Durand3 has attempted to organize systematically the variables involved in hydraulic-solid transport in pipes. He has classified the modes of flow into three types according to the size of the particles in the mixture— homogeneous mixtures, intermediary mixtures and heterogeneous mixtures. With the usual concentrations and flow rates used in hydraulic transportation, particles with diameters of less than 20 or 30 microns form eszentially homogeneous mixtures with water. The data show, however, that even small materials will tend to settle out under laminar flow conditions. Mixtures containing solids over 50 microns in diameter do not achieve total homogeneity even under turbulent flow conditions. Particles from 50 microns to 0.2 mm in diameter may be transported in fully suspended flow at normal transport velocities although the concentration in the vertical plane is not uniform. Above 2 mm in diameter solid materials are transported along the bottom of the conduit at a velocity substantially less than that of the liquid itself. Between 0.2 and 2 mm in diameter, the particles tend to be in a transition zone between heterogeneous suspended flow and deposit flow at normal hydraulic transport velocities. The sand sizes used in fracturing usually fall in this size range. It is interesting to note that the grain size range designated by Durand for this transition zone corresponds closely to the transition zone between

By M. Khorouzan, L. Thomas

Designers of semiconductor devices have been strivi,ng to resolve problems associated with Au-A1 alloys in bonded in.tercomzeclions. One approach now being- used is that of waintaining a physical seyav-atioz between the two metals in bond areas. This is accolrzplished by alunzincnz-plating a bonding area on the tips oJ the kovar leads and using alcminurn wires to join the senzicondictor device to the leads. The portion of the kovar lead which is on the externul side of the sealed package is gold-plated to provide an oxide-free surface for soldering or welding. A discoloration condition originally thought to be sinilar to purple plague, occuving in the yluled uluninur bonding area after package sealing, has been investigated to determine its efiects ipm bond integrity. Electron-micro-probe analysis determined that no1 only gold, but lead, zinc, and silicon were also present in the discolored area. A series of samples conlaining' conkrolled umonts of these inzpitrities weve prepared and subjected to a sil.zuluted sealing process. The investigations swcued that, of the contawiinants, only zinc toas detrinenlul to Lhe bond integily. The discoloration condition itself was found not to be detrimental to the bond integrity. DESIGNERS of semiconductor devices have been striving to resolve problems associated with Au-A1 alloys in bonded interconnections. One approach now being used is that of maintaining a physical separation between the two metals in bond areas. This is accomplished by aluminum plating a bonding area on the tips of the kovar leads and using aluminum wires to join the semiconductor device to the kovar leads. The portion of the kovar lead which is on the external side of the sealed package is gold-plated to provide an oxide-free surface for soldering or welding. Contamination as evidenced by discoloration of the aluminum-plated area was observed in a number of integrated circuits undergoing examination for defect characteristics which cause electrical failures.' This paper contains the results of an investigation to determine the nature of this discoloration, its cause, and its effect upon the integrity of the interconnection bond. I) THE NATURE AND EXTENT OF ALUMINUM-BOND CONTAMINATION The initial hypothesis in the investigation was that the discoloration was caused by reaction of the aluminum film with some unknown contaminants during the sealing of the hermetically sealed integrated-circuit flat package. The package is a rectangular ceramic container sealed with glass which surrounds the kovar leads as well as joining the top to the bottom. The seal is made hermetic by heating and cooling the package to devitrify the glass. In the case of the packages under investigation, the hermetic sealing had been accomplished with dry air as internal atmosphere. The apparent effect of contaminations as observed by microscopic examination was the formation of surface oxides having variations in color encompassing the whole spectrum of visible light. The contamination appeared to be related to one of the more notorious examples of these colorations, the so called purple plague.' In addition to purple plague, Fig. 1 shows the tarnish in the luster of the aluminized surface in the bond area which had been observed in many of the integrated circuits. To identify the contaminant in the bond area electron-probe microanalysis techniques were used.3 Fig. 2 shows the result of this analysis. The contaminants identified were gold, aluminum, zinc, lead, silicon, and cobalt. Fig. 2(a) is a back-scatter display of the area under study. The back-scattered electrons provide a general indication of the distribution of elements in the specimen surface. Elements with higher atomic number scatter more electrons back from the surface and are seen as light areas in the picture. The sample current, Fig. 2(b), is the amount of current conducted by the specimen as a result of electron-beam striking it and is an indication of element distribution. The Sample current is the reverse of back-scatter and complements it. Other pictures in Fig. 2 are produced by characteristic X-rays generated by the elements, allowing the isolation of the element of interest. The isolated element appears white and all other elements are dark. In this manner a comparative study provides a correlation between different surface areas and the elements which are in these areas. The area covered by the gold film, Fig. 2(c), shows that the boundary between the gold film and the kovar is not sharp as expected and that some sort of diffusion has taken place. Fig. 2(c) shows that some gold particles have been carried to the bond area and are in the proximity of the bonded wire in spite of the presence of a physical barrier in the form of the un-

Jan 1, 1967

By G. P. Airey, R. F. Mehl, T. A. Hughes

The coarsening of cementite particles in a ferrite matrix has been studied in a series of steels with 0.15 pct C only and 0.15 pct C plus 1 pct Ni, Mn, and Cr, respectively. Two initial states were employed: quenched nartensite, and quenched and cold-rolled martensite. A series of tempering temperatures between 500' and 700" and tempering times of up to 190 hr were used. The structures were studied by replica and transmission electron microscopy. Particle size distribution curves were determined. From the average size value coarsening curves were obtained. These were plotted in accordance with the Wagner analysis assuming diffusion control. A discussion of the significance of the results is given. L HE reactions occuring upon the tempering of martensite have long engaged the attention of metallurgists. The latter stages, when cementite particles coarsen in a ferrite matrix, have been studied both qualitatively and quantitatively. Studies of such coarsening processes have recently been spurred by the publication of the Lifshitz-Wagner theory1, and the extension of this to the a Fe-Fe3C system by Oriani3 and by Li, Blakely, and einold. Following Wagner the coarsening process is often designated as "Ostwald Ripening". The only quantitative data on the rate of coarsening, except for the work of Hyam and uttin,' in the a Fe-Fe3C system are those of Bannyh, Modin, and odin' for a commercial eutectoid steel and those of Heckel and ereorio" using a pure eutectoid steel. The data of Bannyh, Modin, and Modin have been employed by 0riani3 to derive the a Fe-FeE interface energy. The reaction is one of the most important ones in steel and is worthy of detailed study. This is the purpose of the present study. Laboratory heats were prepared; these were steels with approximately 0.15 pct C, selected so that the num ber of carbide particles would be relatively small and thus so that the overlapping diffusion fluxes would be minimized, presumably a desirable circumstance.'-3 In addition to Fe-C alloys, comparable heats containing 1 pct of Ni, Mn, and Cr, respectively, were included with a view of appraising the effect of alloying elements. This report includes an account of the micro-structures observed, primarily with the electron microscope, and of kinetic data and their interpretation. MATERIALS AND TREATMENT The alloys were prepared from electrolytic iron ("Plastiron") and high-purity graphite; these were melted in a zirconia crucible using a vacuum furnace. The alloy steels were made by adding electrolytic nickel, electrolytic manganese, and "vacuum grade" chromium, respectively, under a partial pressure of argon. Each melt was poured into a mold within the vacuum furnace and cooled in the mold. The ingots were 2 in. in diam. and 8 to 10 in. long. The analysis of the alloys is given in Table I. These ingots were hot-rolled to strip 0.1 in. thick, then cold-rolled to 0.05 in. and each alloy split into two batches. One batch was austenitized at 1200 for 1 min, quenched in cold brine, then cold-rolled to 0.02 in.; samples given this treatment are hereinafter designated as "worked". The other batch was cold-rolled to 0.025 in., austenitized at 1200" for 1 min, and quenched in cold brine; such samples are hereinafter designated as "quenched". These two batches were then tempered, as below. The purpose of the treatment given the first batch was to provide an initial structure of cold-worked martensite, with the expectation that the additional defect structure created by cold work would encourage a higher rate of nucleation of cementite on tempering and hence a more uniform distribution of cementite particles. Individual specimens were sealed in evacuated quartz or Pyrex tubes, then tempered in a muffle furnace. The temperature control was better than 3'C at 700. Tempering treatments wer: performed at 400°, 500°, 550°, 600°, 65o°, and 700C for time periods between 15 min and 190 hr. PREPARATION OF SPECIMENS Specimens for optical and replicalelectron microscopy were mounted, polished conventionally, and etched with 2 pct nital. For electron microscopy, single-stage "formvar" replicas were made, dry-stripped and rotary-shadowed with chromium at an angle of 30 deg. Carbide extraction replicas were prepared from electropolished specimens usirig the method described by Smith and uttin.' Thin foils for electron transmission microscopy were prepared by chemical thinning in an H202-HF bath prior to electropolishing in a chromium trioxide-acetic acid solution. The most

Jan 1, 1969

The Institute would he glad to purchase from any Member a copy of the Bulletin for May, 1914.

Jan 5, 1917

By Edward W. Parker

This plant was built in 1907 at the Bankhead mines to manufacture briquettes by the Zwoyer process under license from the Zwoyer Fuel Co., of New York, N. Y. The building was constructed to contain two units, each of a capacity of 10 tons per hr.; one unit was installed at the time the building was constructed, and the second unit is now being built. The coal used is an anthracite, which is more friable than that of Pennsylvania, and, as a consequence, a larger percentage of dust or waste is produced, which was formerly thrown upon the slack-pile as waste, but is now passed to the ? dust-bin " in the breaker, from which it is conveyed to the briquette-plant.

Jan 5, 1908

By V. J. Berry, J. D. Pendergrass

Well pressure transient tests provide a means for directly obtaining information about formation pressure and reservoir flow capacity. Such tests have also been proposed for determining presence and location of faults or other reservoir closures and for measuring oil in place. For mathematical convenience, most theoretical studies have considered the reservoirs to be homogeneous. Definitive information is not yet available to show whether the actual presence of nonuniformities will make pressure transient behavior different from that of a uniform reservoir. The conclusions reached from actual transient tests are questionable, therefore, insofar as they rely on the original assumption of homogeneity. One type of nonuniformity commonly assumed to exist is that of stratification. In most reservoirs the strata are thought to be in vertical communication. Equations for the transient flow of a single-phase, compressible fluid in a one-well, bounded, circular reservoir have been solved for several situations involving crossflow between multiple strata of various thicknesses and permeabilities. The results show that except for the very early flow period, which usually is too short to be analyzed, the transient performance observed at the well is substantially identical with that of a homogeneous reservoir having the same dimensions and having the same steady-state flow capacity. Thus, stratification does not adversely affect interpretation of well transient tests. This conclusion holds for all commonly encountered combinations of reservoir thickness and external radius. Deviations are observed for unusually thick reservoirs whose outer radii are relatively small. The results of these studies also show that the presence and the amount of stratification cannot be simply diagnosed from reservoir pressure transient data when there is crossflow between strata. INTRODUCTION The last decade has brought wide acceptance of the transient well pressure test for determining reservoir parameters. Following the original work of Hurst and van Everdingen,1 the mathematical theory was thoroughly explored. Numerous authors have suggested how to determine static reservoir pressure, permeability-thickness product, original oil in place and reservoir limits for different reservoir geometry. The same mathematical techniques have been used to predict the transient performance of a reservoir over a long period of time. Most of the theoretical work has been for homogeneous, isotropic systems. Some results have also been presented for a homogeneous, anisotropic reservoir.2 Petroleum reservoirs are not homogeneous. The deposition process seems to favor creation of a stratified formation. This concept is sufficiently well accepted so that the most natural extension of the transient flow theory beyond the homogeneous case is to a stratified formation. Results for a stratified reservoir with no vertical communication between layers can be obtained from the results for a homogeneous reservoir. Lefkovitz, et a1,3 have given a thorough treatment of the two-layer case. Two recent papers4,5 have treated the case of a two-layered reservoir with vertical communication or crossflow, between layers. Russell and Prats4 find that, after a relatively short time, the two-layered reservoir with crossflow exhibits a simple exponential pressure decline. From this time forward, the behavior is not distinguishable from the behavior of a homogeneous reservoir having the same steady-state flow capacity. The results of Katz and Tek 5 are equivalent. Russell and Prats4 also speculate that a multi-layered reservoir with crossflow will behave as a homogeneous system after long enough production time "... providing the contrast in kh between layers is not too great". They also suggest that, at intermediate times, "... the relative positions of the layers with respect to each other will have a great influence on the production behavior and on the time at which the previously mentioned large-time approximation might be valid". Katz and Tek5 remark upon the mathematical difficulty of treating a reservoir having many layers or strata. If relative position of the layers is also

By V. C. Allison

The explosibility of a dust is favored by its fineness and content of volatile combustible matter; its explosibility is decreased by its moisture and ash content. The explosibility of a dust can be reduced by admixture of either inert dust or water. The major effect of both the inert dust and water lies in their heat capacity; they absorb the heat of the explosion flame until the temperature of this flame drops below the ignition temperature of the explosive heat. The amount of inert dust necessary to make an explosive dust non-explosive can be calculated from its proximate analysis. FOREWORD LARGE-SCALE testing of the explosibility of coal dust as conducted by the Bureau of Mines in its Experimental Mine involves a large initial investment, and a high charge for maintenance and conduct of the test; in addition the work is necessarily slow because of the time required for the preparation of the tests and the cleaning and repairing of the mine after each test. These tests have been made along practical mining lines that admit of a range of mixtures of dust varying from 5 to 10 per cent. and with gas as low as 0.5 per cent. increments. Because of the time and expense involved, efforts have been made to devise a type of gallery for laboratory use in which the results obtained in the Experimental Mine may be correlated as an aid in a study of dusts, the explosibility of which might be approximately determined quickly and at a minimum of expense. The explosibility of coal dust has been studied by a number of European investors, using small laboratory devices; among these may be mentioned the experiments con¬ducted by Galloway, Vital, Hall and Clark, Abel, Mallard and Chatelier, Thorpe, Bedson and Widdas, Engler, Holwartz and Meyer, and Taffanel, results of whose experiments have been reviewed by the Bureau of Mines., The Bureau has conducted many tests with the Frazer-Clement2 apparatus, which gives the pressures set up when the dust cloud within is, ignited with a platinum coil or tube, heated to different temperatures, but for these tests the sample must be especially prepared as to size (200 mesh) and must be dry. An attempt has been made to design an apparatus that may be used for checking and correlating the experimental tests. The first design was a wooden gallery, 8 by

Jan 7, 1925

By Ancel St. John

During a session on coal and coke at the February, 1926, meeting of the American Institute of Mining and Metallurgical Engineers, the writer called attention to the important work on the X-ray analysis of coal1,2 being carried on in England by C. Norman Kemp and his associates. This aroused so much interest that a paper on the subject was requested for the October meeting. It has seemed advisable to make this paper a preliminary survey of the present status in the application of X-ray methods to coal problems and to follow it from time to time with further articles as the art develops. A survey of this sort naturally divides itself into two parts, radio-scopic analysis of the distribution of constituents through the body of the coal, and diffraction analysis of the state of association of the elementary components. In this article the subject matter concerning radioscopic analysis has been drawn almost entirely from the writings of Kemp and his associates and the illustrations have been sptcially furnished by him. It is a pleasure to record here a great indebtedness for this courtesy and cooperation. The subject matter and illustrations concerning diffraction analysis are taken from the author's unpublished researches. Nature and Properties of X-rays Before proceeding it is well to recall the nature and some of the properties of X-rays, as well as our present conception of atomic structure According to the accepted theory atoms are composed of electrically-charged particles. A positively-charged center, called the nucleus,

Jan 1, 1927