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By John B. Baker, Bernard B. Betty, H. F. Moore

For several years there has been in progress in the Materials Testing Laboratory of the University of Illinois an investigation of creep and fracture of lead and lead alloys. In the course of this investigation it has been shown that the phenomenon of creep occurs in part at the grain boundaries of lead and lead alloys. To study the occurrence of creep and the development of fracture within crystalline grains, two series of tests of single crystals of lead have been carried out. The first of these, a preliminary series, by Mr. Betty, has been described.l,2 The second, pursued by Mr. Baker for his doctoral dissertation, was carried out under the direction of Professor Moore, with the assistance of Prof. G. L. Clark in the X-ray work, and the cooperation and advice of Mr. Betty. This paper is based on the test data obtained in this second series. Single crystals of a very pure commercial lead have been prepared, some of them tested to measure creep, others tested to fracture under long-continued steady load, and still others tested under cycles of repeated tension. An interpretation of the test data of these single-crystal tests is offered, which is a combination of parts of several well-known theories. Specimens The single-crystal specimens were made from a piece of very pure commercial lead sheathing. A spectroscopic analysis of one of the single crystals showed the presence of 0.005 per cent Bi, 0.0001 per cent Cu and 0.0003 per cent Ag. Preparation.—The Bridgman method of casting single-crystal specimens was used.3 The specimens were cast to the shape and size shown in Fig. 1 (dimensions in Fig. 4c) in a duralumin mold. Molten lead does not stick to duralumin. Fig. 1 shows the mold and the blast flames for heating. After the mold had been heated to the temperature of molten

Jan 1, 1938

By Maurice Ewing, J. A. Peoples, J. W. Peoples, A. P. Craby

The purpose of this paper is to present the results of the application of the earth-resistivity method of subsurface investigation to the problem of locating seams of anthracite coal beneath a mantle of soil and subsoil. Details are given of the successful use of this method in locating the outcrops of anthracite seams in actual prospecting. The presence of the outcrop of an anthracite seam is indicated at points where electrical resistivity tests showed relatively low readings. The reason for this is that in some localities the resistivity of anthracite was found to be about 0.0001 megohm-cm. compared to 1 to 200 megohm-cm. for shales and sandstones. For two reasons it is believed that the data summarized in this paper should be of particular interest. In the first place, most of the interpretations of the resistivity survey have been checked by subsequent drilling and some by the removal of the overburden and the exposing of the anthracite seams. It is infrequent that the opportunity for checking results so thoroughly is given. In the second place, the fact that recent commentatorsl,2,3 on the application of geophysical methods to mining have concluded that direct prospecting for anthracite and other types of coal is not promising makes the good results obtained more significant. So far as the authors can learn, the only previous experiment with electrical methods in the Pennsylvania anthracite field was one made by Sherwin F. Kelly in 1921, when he used the self-potential method at Wilkes-Barre4. The profile he made does not show a very marked correlation with the geologic cross section. Kelly points out that stray currents from electric motors in the mines undoubtedly affected 'his results, but the experience of the present authors with stray currents from mining machinery suggests the possibility that the potentials measured by Kelly were due almost entirely to this effect.

Jan 1, 1936

THE metal iron has physical and chemical properties which are somewhat different from those of steels, but a knowledge of the pure metal is a useful starting point in studying the behavior of steels. Solid iron exists in two different crystalline forms, called alpha (a) and gamma (?) iron, the former being the ordinary form at room temperature. When heated above the "A2 point," 768 C (1414 F), the metal becomes nonmagnetic, and at the "A, point," 910 C (1670 F), it undergoes a change in crystalline form to become gamma iron. In the range 768 to 910 C, it is sometimes called beta (ß) iron to distinguish it from the magnetic alpha, but the two are identical in crystal structure. When gamma iron is further heated to 1400 C (2552 E), it changes into delta (d) iron, which is identical with beta or non- magnetic alpha iron. Pure iron melts (in an inert atmosphere) at 1537 C (2800 F); the melting point is generally lowered by alloys or impurities. PROPERTIES OF IRON AT HIGH TEMPERATURES Many of the properties of iron undergo abrupt changes at the transition temperatures.1 For example, in heating through the A, point, a sudden shrinkage in volume occurs. Similarly, melting is attended by sharp physical changes such as an increase in volume. Table 16-1 contains a summary of the measured physical properties of pure iron at several temperatures. Usually the properties change smoothly within the range of stability of a given form, but this is not always true. For example, the specific heat reaches a sharp maximum at the A2 point although no trans- formation occurs. (See Fig 14-1.) Solvent Powers of Liquid Iron. Liquid iron is capable of dissolving most of the other metals and many nonmetallic elements as well. Of the metals that are liquid at the melting point of iron, only lead, silver, and bismuth refuse to dissolve to an ap-

Jan 1, 1951

By Maurice Ewing, A. P. Craby, J. W. Peoples, J. A. Peoples

The purpose of this paper is to present the results of the application of the earth-resistivity method of subsurface investigation to the problem of locating seams of anthracite coal beneath a mantle of soil and subsoil. Details are given of the successful use of this method in locating the outcrops of anthracite seams in actual prospecting. The presence of the outcrop of an anthracite seam is indicated at points where electrical resistivity tests showed relatively low readings. The reason for this is that in some localities the resistivity of anthracite was found to be about 0.0001 megohm-cm. compared to 1 to 200 megohm-cm. for shales and sandstones. For two reasons it is believed that the data summarized in this paper should be of particular interest. In the first place, most of the interpretations of the resistivity survey have been checked by subsequent drilling and some by the removal of the overburden and the exposing of the anthracite seams. It is infrequent that the opportunity for checking results so thoroughly is given. In the second place, the fact that recent commentatorsl,2,3 on the application of geophysical methods to mining have concluded that direct prospecting for anthracite and other types of coal is not promising makes the good results obtained more significant. So far as the authors can learn, the only previous experiment with electrical methods in the Pennsylvania anthracite field was one made by Sherwin F. Kelly in 1921, when he used the self-potential method at Wilkes-Barre4. The profile he made does not show a very marked correlation with the geologic cross section. Kelly points out that stray currents from electric motors in the mines undoubtedly affected 'his results, but the experience of the present authors with stray currents from mining machinery suggests the possibility that the potentials measured by Kelly were due almost entirely to this effect.

Jan 1, 1936

By R. K. Hopkins

For a great many years fusion welding has been used in and around petroleum refineries, but it is only within six or seven years that the more important pressure vessels have been constructed by this process, because before that time the properties of fusion welds would not with-stand such rigorous service. Since the adoption of fusion welding for the construction of this equipment, the refiner has required pressure vessels suitable for operation over a very wide range of conditions. On the one hand, vessels must operate at extremely high temperatures, in the range of 950° to 1000° F., and on the other vessels must be suitable for operation at sub-zero temperatures down as low as -75° F. Also, vessels are required suitable for operation at pressures upwards of 1000 lb. per sq. in., and as low as a 29-in. vacuum. In addition, vessels are required to withstand the attack of very corrosive mediums. It has been a rather difficult task for the fabricator to meet all of these require-ments, but as a result of the extensive research carried on by steel manu-facturers and several fabricators of class I vessels, practically all of these demands have been met. In order to meet the refiners' requirements for this wide range of conditions, the fabricator has worked closely with the metallurgist. This has enabled him to choose the proper base metal for each service condition, but it has been the fabricator's problem to develop a welding rod and welding technique, as well as a heat-treatment, that would produce in the welded vessel characteristics in and around the weld comparable to those in the base metal. Where corrosion is not a serious problem, and where the operating temperatures are not too high, ordinary carbon steel has served very well. But when corrosion is serious, and/or when the temperatures are either very high or very low, it is necessary to use some form of alloy steel to give satisfactory service.

Jan 1, 1935

By W. R. Shimer

IN his valuable report on Finishing Temperatures and Properties of Rails, I Dr. G. K. Burgess, Chief of the Division of Metallurgy, U. S. Bureau of Standards, has begun a line of investigation which should be continued by those interested in the subject, and who have proper facilities for carrying put the work. For the past year or more the Bethlehem Steel Co. has been conducting experiments to learn the effect of rail finishing temperatures on their physical properties and microstructure and the results are here given for the consideration of those interested in the rail situation. . Considerable differences of opinion have been expressed by various authorities, in the past, as to the effect of large or small grain size and high or low finishing temperatures of steel rails on their physical properties and wearing qualities. Low finishing temperatures and, therefore, low shrinkage, have been advocated on the theory that the wearing qualities would be improved. Others have recommended high finishing temperatures. The generally accepted cause for rail failures, due to the development ,of transverse fissures, is excessive wheel pressure on hard rails. One of the causes advanced for hard rails has been that they contain too high per centages of carbon and manganese; another that the rails were finished at too low a temperature, i.e., at or near the critical point. In the experiments herein described the rails were rolled from reheated blooms. All the rail blooms were charged hot in a reheating furnace and brought up to about the original ingot-rolling temperature before rolling into rails. These rails gave better results in deflection, withstood a greater number of drops before breaking, and showed greater ductility, than. rails of identically the same composition and section which were rolled, direct from the ingot. Rails rolled from reheated blooms, finished at somewhat higher temperatures than when rolled direct from the ingot, have a different microstructure, which the writer does not believe is due so much to the difference in finishing temperatures, as to the difference in

Jan 3, 1915

By R. K. Hopkins

For a great many years fusion welding has been used in and around petroleum refineries, but it is only within six or seven years that the more important pressure vessels have been constructed by this process, because before that time the properties of fusion welds would not with-stand such rigorous service. Since the adoption of fusion welding for the construction of this equipment, the refiner has required pressure vessels suitable for operation over a very wide range of conditions. On the one hand, vessels must operate at extremely high temperatures, in the range of 950° to 1000° F., and on the other vessels must be suitable for operation at sub-zero temperatures down as low as -75° F. Also, vessels are required suitable for operation at pressures upwards of 1000 lb. per sq. in., and as low as a 29-in. vacuum. In addition, vessels are required to withstand the attack of very corrosive mediums. It has been a rather difficult task for the fabricator to meet all of these require-ments, but as a result of the extensive research carried on by steel manu-facturers and several fabricators of class I vessels, practically all of these demands have been met. In order to meet the refiners' requirements for this wide range of conditions, the fabricator has worked closely with the metallurgist. This has enabled him to choose the proper base metal for each service condition, but it has been the fabricator's problem to develop a welding rod and welding technique, as well as a heat-treatment, that would produce in the welded vessel characteristics in and around the weld comparable to those in the base metal. Where corrosion is not a serious problem, and where the operating temperatures are not too high, ordinary carbon steel has served very well. But when corrosion is serious, and/or when the temperatures are either very high or very low, it is necessary to use some form of alloy steel to give satisfactory service.

Jan 1, 1935

By Herbert Hoover

THE desire of the engineers over the last few years, growing out of their contact with public affairs, that this Institute should take a wider vision than the narrower field of technology and should apply its skill to the development of civic problems which must lay in their foundation on engineering, has led to this discussion today. Some of us in San Francisco, in discussing this question of the relation of the engineers to civic problems, raised the question as to whether or not in this national emergency it was not the duty of the Mining Engineers to bring, forward their combined skill and knowledge and experience to bear upon the problems of the coal industry. This industry, considered as a whole, is one of the worst functioning industries in the United States. It is equipped with capital, with machinery, plants and labor to a peak load at least 20 per cent. above the average necessity. This peak load, therefore, involves the use of probably 100,000 men diverted from other productive industries; it involves an intermittency of employment through its whole personnel that results not only in a long train of human woe, but results also in a higher cost of coal -to the general public. The problem of whether the industry can, by any device, be cured or even partially cured of its intermittency, is solely an engineering problem. It is therefore an apropos problem for this Institute. Your President and myself and others thought that we could best develop this discussion by calling upon men of large experience in the particular branches of the soft coal industry, to bring the facts in front of this general committee, with a view to an exhaustive discussion and perhaps subsequently the appointment of a committee to formulate those facts and such remedies as may be developed into a report that would be of constructive value.

Jan 3, 1920

By R. K. Hopkins

Fox a great many years fusion welding has been used in and around petroleum refineries, but it is only within six or seven years that the more important pressure vessels have been constructed by this process, because before that time the properties of fusion welds would not withstand such rigorous service. Since the adoption of fusion welding for the construction of this equipment, the refiner has required pressure vessels suitable for operation over a very wide range of conditions. On the one hand, vessels must operate at extremely high temperatures, in the range of 950° to 1000° F., and on the other vessels must be suitable for operation at sub-zero temperatures down as low as -75° F. Also, vessels are required suitable for operation at pressures upwards of 1000 lb. per sq. in., and as low as a 29-in. vacuum. In addition, vessels are required to withstand the attack of very corrosive mediums. It has been a rather difficult task for the fabricator to meet all of these requirements, but as a result of the extensive research carried on by steel manufacturers and several fabricators of class I vessels, practically all of these demands have been met. In order to meet the refiners' requirements for this wide range of conditions, the fabricator has worked closely with the metallurgist. This has enabled him to choose the proper base metal for each service condition, but it has been the fabricator's problem to develop a welding rod and welding technique, as well as a heat-treatment, that would produce in the welded vessel characteristics in and around the weld comparable to those in the base metal. Where corrosion is not a serious problem, and where the operating temperatures are not too high, ordinary carbon steel has served very well. But when corrosion is serious, and/or when the temperatures are either very high or very low, it is necessary to use some form of alloy steel to give satisfactory service.

Jan 1, 1935

By Paul M. Tyler

Mineral raw materials, because they are essential to our industrial prosperity and military strength, must be made available in substantial quantities. regardless of cost. Variations in the cost of procuring minerals, as compared with the cost of obtaining other commodities, and changes in the cost of production of different minerals relative to one another, will naturally influence the quantities of a given mineral item that can be marketed readily. However, in the last analysis, the cost of winning minerals from the ground usually constitutes only a small fraction of the value of the end-use products and services derived from them. The miner's share of the cost of a typewriter, telephone circuit, or even a modem office building, is almost insignificant. Far more important to the ultimate consumer, therefore, than any minor saving in cost is the assurance of ample supplies of the minerals needed to aliment our expanding economy. To create a successful metal mining operation involves ( 1 ) the discovery and systematic development of a mineral deposit, (2) extraction of the ore, (3) the mechanical and metallurgical processing to eliminate worth- less or harmful impurities, and (4) the profitable disposal of the product. The first step of the technological process belongs chiefly in the realm of the geologist, the second is a mining engineer's job, the third is mainly up to the millmen and extractive metallurgists; whereas the fourth and equally important step poses a commercial problem that has aspects in common with the marketing of other products. Ore finding is far from being an exact science. There is no mathematical criterion for evaluating the efficiency of prospecting and exploration. Lady Luck shares the honors or assumes part of the blame along with the prospector and geologist. Marketing like- wise involves factors that seemingly defy engineering analysis. Although the other steps can be measured with some degree of mathematical accuracy, even they tend to vary so widely in basic principle, as well as in

Jan 1, 1959

By Paul M. Tyler

Mineral raw materials, because they are essential to our industrial prosperity and military strength, must be made available in substantial quantities regardless of cost. Variations in the cost of procuring minerals, as compared with the cost of obtaining other commodities, and changes in the cost of production of different minerals relative to one another, will naturally influence the quantities of a given mineral item that can be marketed readily. However, in the last analysis, the cost of winning minerals from the ground usually constitutes only a small fraction of the value of the end-use products and services derived from them. The miner's share of the cost of a typewriter, telephone circuit, or even a modem office building, is almost insignificant. Far more important to the ultimate consumer, therefore, than any minor saving in cost is the assurance of ample supplies of the minerals needed to aliment our expanding economy. To create a successful metal mining operation involves (1 ) the discovery and systematic development of a mineral deposit, (2) extraction of the ore, (3) the mechanical and metallurgical processing to eliminate worthless or harmful impurities, and (4) the profitable disposal of the product. The fist step of the technological process belongs chiefly in the realm of the geologist, the second is a mining engineer's job, the third is mainly up to the millmen and extractive metallurgists; whereas the fourth and equally important step poses a commercial problem that has aspects in common with the marketing of other products. Ore finding is far from being an exact science. There is no mathematical criterion for evaluating the efficiency of prospecting and exploration. Lady Luck shares the honors or assumes part of the blame along with the prospector and geologist. Marketing like- wise involves factors that seemingly defy engineering analysis. Although the other steps can be measured with some degree of mathematical accuracy, even they tend to vary so widely in basic principle, as well as in

Jan 1, 1964

By H. S. Rawdon

One of the most vital problems in the manufacture of steel at present is the occurrence of the defects that have been popularly termed "snow flakes," "flakes," or "scabs." Particularly is this the problem of many manufacturers who, during the past 2 yr., have undertaken large-scale production for the first time. A study of the microstructure of such defective material throws considerable light upon the nature of these defects and is essential before measurcs may be taken for the elimination of the defects. Flakes do not appear to be found in the plain carbon steels; they have been found. however, in abundance in some of the simple alloy steels that are being used in such vast quantities; vie., nickel steel of the approximate composition, 0.40 carbon and 3.5 per cent. nickel, and in the chrome-nickel type. The present article summarizes the characteristic features of defective steel of the flaky type as they have been found by laboratory study of numerous specimens, and it aims to show the conditions within the metal that are favorable to the occurrence of this type of defect without entering into the details of mill practice (size of ingot, design of molds, rate of cooling, distribution of cooling stresses, etc.), all of which conditions appear to play a role in the production of these defects. MacrostrUctURe To one familar with flaky steel, the appearance of "snow-flakes" is unmistakable and is not to be confused with other types of defects. Figs. 1 to 6 show the appearance of fractures of steel showing this type of defect; the white silvery area, which always has the appearance of being of a very coarsely crystalline structure, in the specimen stands out in bold contrast to the darker background and readily justifies the use of the term "snow-flakes." Fig. 1 shows the appearance of the faces of the two halves of a nickel-steel forging that has been split to show the interior flakes. Fig. 2 is a nickel-steel bar (carbon 0.40 per cent.,

Jan 1, 1920

By Edgar C. Bain, William E. Griffiths

The results of an inquiry into the structural nature of some 70 iron alloys containing both nickel and chromium over a considerable range of concentration are briefly described in this paper. This study is a part of a comprehensive program of investigation into alloys involving chromium in progress at the Union Carbide and Carbon Research 1aboratories. All the compositions studied contained carbon in amount comparable to commercial alloys. The B Constituent In addition to locating the limits of composition for the three principal types of structure (polyhedral ferrite, martensite and austenite) and their combinations, certain other features of the system were observed. A hitherto undescribed brittle constituent (designated here as the "B constituent") was discovered. It is very hard, non-magnetic and forms in two modes from chrome-ferrite by recrystallization. It is the stable low-temperature condition for the equal-proportion chromium-iron materials containing less than 10 per cent. nickel. Although it partakes of the nature of an inter-metallic compound, yet it may exist over a considerable range of composition. It is non-existent above a temperalure zone, varying with composition, from 800° C. to 950° C., and heating above this critical temperature develops chrome ferrite persistent after average cooling rate; a few hours just below this temperature will develop the complicated brittle crystalline type. The B constituent, when found in the grain boundaries of alloys of lower chromium content, contributes a serious brittleness removable, however, by heating and cooling rapid enough to prevent its re-format'ion. By suitable means of precipitution, the hard B constituent can be made to strengthen the already stiff alloy matrix in the manner of submicro-scopic particles, as exemplified in duralumin or the Sykes iron-tungsten and iron-molybdenum alloys. A possible explanation is offered for the familiar brittleness developed in chrome iron at temperatures above about 475" C. and removable by

Jan 1, 1927

By W. R. Shimer

In his valuable report on Finishing Temperatures and Properties of Rails,l Dr. G. X. Burgess, Chief of the Division of Metallurgy, U. S. Bureau of Standards, has begun a line of investigation which should be continued by those interested in the subject, and who have proper facilities for carrying out the work. For the past year or more the Bethlehem Steel Co. has been conducting experiments to learn the effect of rail finishing temperatures on their physical properties and microstructure and the results are here given for the consideration of those interested in the rail situation. Considerable differences of opinion have been expressed by various authorities, in the past, as to the effect of large or small grain size and high or low finishing temperatures of steel rails on their physical properties and wearing qualities. Low finishing temperatures and, therefore, low shrinkage, have been advocated on the theory that the wearing qualities would be improved. Others have recommended high finishing temperatures. The generally accepted cause for rail failures, due to the development of transverse fissures, is excessive wheel pressure on hard rails. One of the causes advanced for hard rails has been that they contain too high percentages of carbon and manganese; another that the rails were finished at too low a temperature, i.e., at or near the critical point. In the experiments herein described the rails were rolled from reheated blooms. All the rail blooms were charged hot in a reheating furnace and brought up to about the original ingot-rolling temperature before rolling into rails. These rails gave better results in deflection, withstood a greater number of drops before breaking, and showed greater ductility than rails of identically the same composition and section which were rolled direct from the ingot. Rails rolled from reheated blooms, finished at somewhat higher temperatures than when rolled direct from the ingot, have a different microstructure, which the writer does not believe is due so much to the difference in finishing temperatures, as to the difference in

Jan 1, 1915

By Larry Kaufman, Joan B. Berkowitz-Mattuck, Edward V. Claugherty

The oxidation characteristics of hafnium and zirconiunr diboride were measured between 1200 and 2200'K by a thermal- conductivity method which continuously ttzeasures the rate of reaction of oxygen with the diboride and by a metallographic air oridation method zuhich provides a measure of the total arr7ount of bovide conuerted to oxide for a given time interval. The oxidized specimens obtained from the tl~eritaal-coi~ductitrity method were also examined by quantitatire metal-lographic procedares. The significant results obtained in this investigation reveal that metal-rich compositions of lzafi~iutil diboride proride the most oxidation-resistatzt material up to 2000°K; hafnium diboride is tmre oxidation- resistant titan zirconium diboride at all tempevatures examined; the morphology of the oxide formed on H/B2 and Llie temperature coefficient qi. the oxidation rate constants change at the temperature of ttze monoclinic to tetragonal phase transition] in HfO2; the oxidation of neither HfB2 nor ZrB2, results iN catastrophic Jazlure at lorc. oxygen pressures; and pvefevetztial gvaLti boundary oxidation was not obsevued for either HfBi or ZYB, A comprehensive study of the high-temperature characteristics of refractory transition-metal di-borides is currently in progress. This program has included investigation of the physical, thermal, and thermodynamic properties of TiB2, ZrB2, HfB2, NbB2, and TaB2. In addition, aspects of the synthesis and fabrication of such materials have been studied. In view of the diverse nature of this research, a number of other laboratories have actively participated and contributed specific capabilities for analysis and characterization of these materials. As a consequence, an extensive description of the relevant properties of these compounds has emerged which is central in evaluating their high-temperature (1200" to 2500°K) performance. To date, information on thermodynamic stability, specific heat, and vaporization characteristics,1 hot hardness and electrical resistivity,1, 3 therma1 expansion:'4 and thermal conductivity 1, 5 has been presented. This information has been generated on materials of the highest purity (98.5 to 99.9 wt pct Me + B) and density currently available. Samples fabricated by zone melting6 and high-pressure hot pressing"3'7 techniques have been used to generate suitable specimens for all of the aforementioned studies. dation characteristics of the most oxidation-resistant of these materials, hafnium and zirconium diboride, is presented and a description of the synthesis and the experimental procedures used to prepare and characterize specimens is given. The high-temperature range under consideration (1200" to 2200°K) and the known dependence of oxidation characteristics on sample chemistry, density, and oxidation conditions required a close coupling of the synthesis, fabrication, and evaluation procedures.8 This was accomplished by continual surveillance of chemical composition of starting materials before and after specimen fabrication and by evaluation of density, phase constitution, and microstructural features prior to and after oxidation exposure. I) PROCUREMENT AND CHARACTERIZATION OF STARTING MATERIALS In view of the current state of the art in fabricating refractory boride materials, the methods used in preparing samples for the present study are given in detail as follows: starting materials were purchased in high-purity powder form and fabricated by high-pressure hot pressing into 0.40 by 1.00 in. bars from which oxidation specimens were obtained. The hafnium diboride used in this study was purchased from Wah Chang Corp.; the zirconium diboride from U.S. Borax and Chemical Co. These powders were routinely characterized by quantitative chemical analyses for metal, boron, carbon, oxygen, nitrogen, and iron, by qualitative emission-spectrographic analysis for trace impurities, by X-ray procedures for extraneous phase identification, and by powder densitometry for comparison with X-ray (theoretical) density. Hafnium and zirconium metal and elemental boron were also purchased as high-purity powders and characterized for impurities by emission-spectrographic analyses. The hafnium diboride was procured in three shipments which were designated as HfBl.g7(1), HfB1.88(2A), and HfB2.12(2). The indicated stoichiometry is based on the atomic ratio of total boron to total hafnium; the number in parentheses identifies the shipment number. Shipment 1 was 5 1b, shipment 2A, 1 1b, and shipment 2, 8 1b. The zirconium diboride was procured as a 20-1b shipment and designated as ZrB1.89(1). A small quantity of purified zirconium diboride was also supplied and designated ZrB1, 9(P). The averaged results for chemical analyses which were generally performed according to the procedures set forth in the compilation by KrieGe9 are presented in Table I. Qualitative spectrographic analyses indicated that Ca, Cr, Ti, Si, Zr (in H~B~), and A1 were present at levels between 0.01 and 0.10 wt pct. Other metallic elements were found to be less than 0.01 wt pct. Since it is virtually impossible to purchase these materials in the desired quantities (5 to 20 lb) as single-phase compounds it is necessary to obtain

Jan 1, 1968

By Frank C. Kelton

It is perhaps not widely realized that extraction and saturation processes carried out on oil well core samples alter the properties of these samples to varying degrees. On the other hand it is felt by some that quick-freezing of core samples increases their permeability and porosity significantly. Accordingly, laboratory tests were carried out on 49 pairs of horizontally adjacent samples in order to differentiate between the effect of quick-freezing per se on permeability and porosity of the samples, as distinguished from the effect of the identical saturation treatment on permeability and porosity of the companion samples. Also, additional field data were obtained on comparison of frozen vs unfrozen companion samples. LABORATORY INVESTIGATION OF FREEZING us SATURATION EFFECTS Procedure The samples used in these tests were two-cm cubes cut in horizontally adjacent pairs from cores from eight Gulf Coast and Mid-Continent wells, which cores had not previously been frozen. These samples were extracted with carbon tetrachloride, dried, and air permeabilities run in the conventional manner. They were then evacuated and saturated with brine of 25,000 ppm sodium chloride content, and porosities determined by gain in weight. The samples were partially desaturated by evaporation down to an average brine saturation of 68 per cent. One sample from each pair was quick-frozen by covering with dry ice after wrapping in a single layer of paper, and allowed to remain frozen for about two hours; the companion sample from each pair was not frozen. After thawing the frozen sample, all samples were immersed in tap water overnight in order to leach out most of the brine. Air permeabilities were re-run, and the samples were again saturated with brine to determine a second porosity value. For purposes of averaging of data, the samples were grouped according to four permeability ranges, from 0 to 10, 10 to 100, 100 to 1,000, and 1,000 to 3,840 md. Average permeability and porosity changes for the frozen vs the unfrozen adjacent samples are shown in Table 1. Discussion As may be seen from Table 1, the averages of the per cent permeability increases for the quick-frozen samples ranged from 3.8 to 12.9 per cent among the four permeability groups. The average changes among the four groups of unfrozen companion samples ranged from a decrease of 0.2 per cent to an increase of 9.3 per cent. There was no particular correlation of these changes with magnitude of permeability; however, the increase for each group of frozen samples paralleled the increase for the corresponding unfrozen samples. The differences between the two sets of values are believed to be a valid indication of the effect of the quick-freezing in itself, since the treatment of the two samples in each pair was identical except for freezing. The permeability changes which are strictly the result of the quick-freezing are shown in the sixth column of Table 1. These range from a decrease of 0.9 per cent to an increase of 4.0 per cent; the overall weighted average is 1.2 per cent, as compared to an average increase of 6.8 per cent caused by the saturation treatment of the samples not frozen. The average porosity changes are in general smaller than the changes in permeability, and range from a decrease of 2.3 per cent to an increase of 3.3 per cent. The overall weighted average change ascribed to the quick-freezing is 1.0 per cent of porosity. Many factors can contribute to the changes in permeability and porosity observed when subjecting cores to the simple processes used in these tests. Such are: hydration and swelling of clay, adsorption of ions, changes in surface structure and wettability, expansion and compression effects due to ice formation, shrinking and cracking, leaching of salts and colloids, displacement of particles resulting in either blocking or enlarging of pore openings. Whatever particular mechanisms are involved. however, it is apparent not only from this study but also from other investigations in the literature' not directly concerned with quick-freezing, that the effects produced by commonly used extraction, saturation and drying techniques may be of considerable magnitude The results of this study indicate that for the particular samples and techniques used, such effects are of the order of five to six times the effect of quick-freezing. insofar as changes in permeability are concerned. It may be argued that these samples might not include extremely shaly material where the effect of freezing upon permeability may be much greater. However, had such material been available for these tests, it would undoubtedly have been very susceptible also to alteration by the extraction and saturation treatment used. To investigate this point further, the individual sample data were re-grouped according to the magnitude of the average per cent permeability increases for the pairs of samples, irrespective of permeability. The results

Jan 1, 1953

By C. L. Prokop

A laboratory investigation has been made of the effects of mud hydraulics upon the formation and erosion of mud filter cakes. The tests were conducted to simulate drilling conditions as nearly as possible. The formation of mud filter cake in a drilling well does not proceed at a uniform and unbroken rate. Instead, the rate of cake accumulation depends upon whether or not the mud is being circulated. If the mud column is quiescent, filter cake formation is a smooth function of the filtration characteristics of the system. If the mud is being circulated filter cake formation depends not only upon the filtration characteristics of the mud but also upon the erosive action of the flowing mud column Filter cakes formed during continuous mud circulation were observed to reach an equilibrium thickness after several hours' circulation. Mud circulation was maintained at a constant volumetric rate throughout each experiment. The fluid velocity at equilibrium cake thickness was dependent upon the thickness of the filter cake. Muds having exceptionally high water loss deposited thick filter cakes in spite of very high eroding velocities. The muds having good filtration characteristics deposited thin filter cakes at equilibrium circulating velocities well within tile range of those in a drilling well. It was observed that filter cakes deposited during stagnant filtration were quite difficult to erode by mud circulation. The - rate of crosion computed from the rate of filtrate accumulation after equilibrium cake thickness had been reached was in reasonable agreement with the rate of erosion obtained by direct observation. Continuous mud circulation usually caused the permeability of the filter cake to decrease with time. INTRODUCTION Many of the difficulties encountered during tile drilling of a well have been attributed to the loss of water from the mud and the attendant deposition of solids upon the walls of the hole. Past experience has shown that a reduction of the filtration rate of the drilling fluid eliminates or greatly reduces these difficulties. Definite filtration requirements, however, are hard to establish for a given set of conditions. This is due. in part, to the fact that the usual filtration test performed upon mud doe? not simulate well conditions as closely as desirable. The filtration characteristics of a mud are customarily determined by means of the standard low-pressure API wall-building tester.' In this instrument a filter cake is deposited upon a horizontal bed under a pressure differential of 100 psi. The rnud is quiescent during the filtration period. In actual practice. mud filtration occurs within a well under quite different conditions. One of the major differences is that mud flows upward across the filter bed as the filter cake forms. This undoubtedly produces a change in the filter cake which cannot be reflected in the results of the API test. The laboratory work described in this paper had as its primary objective a better understanding of the influence of mud circulation upon the thickness and ,characteristics of the filter cakes deposited under conditions similar to those existing in a drilling well. ANALYSIS OF PROBLEM Once a permeable formation is penetrated by the bit, filtrate from the mud flows into the formation. 'he mud solids plaster against the walls of the hole, forming a filter cake. If the mud column is stagnant, that is, if it is not being circulated. the filter cake will increase in thickness until the hole is filled. Prior to the time that the hole is filled, the thickness of filter cake existing at any given time will be a function of the filtration characteristics of the mud, the temperature, and the pressure differential. The effects of these variables have been investigated in the past for both flat bed filtration2'3 and for radial filtration.' When the mud is circulated in a hole in which a filter cake i. being deposited. some of the solids that would ordinarily deposit in the filter cake will be carried away by the eroding action of the mud. This will limit. filter cake thickness. Some work has been done to determine the effect of flow upon the filtration rate in a circulating mud system' but little work has been done upon the factors which determine the filter cake thickness existing in a circulating system. On first sight it would appear that the major factors controlling filter cake formation in a circulating system should be: 1. The rate of deposition of solids from the mud. 2. The erosive force that the flowing mud exerts upon the filter cake. 'A. The erodabilitv of the filter cake. 4. Any change in filter cake characteristics attributable to the scouring action of the mud. The rate at which solids are deposited from the mud will be controlled to a large degree by the filtration characteristics of the mud, the pressure differential. the temperature under

Jan 1, 1952

By Samuel H. Dolbear

THE purpose of a technical report is to record facts, usually collected by investigation, and to interpret these facts in understandable language. The audience may range from a small shareholder without technical knowledge, to a highly trained engineer or geologist. If the client is a mining company with technically trained executives, the report writer's problem is relatively simple. The writer will then be appraised not only for his conclusions, but for clarity of language and organization of the report. If the writing is bad, the construction careless, and there is a failure to clearly convey to the reader the facts and the author's conclusions, the report is a failure and the writer may have damaged his professional character. Spoken words die quickly, written words may constitute a permanent record and if they are badly composed they may rise up to damn the author. "A good measure of an author's understanding of his subject is his ability to express it clearly in plain words." Good English Teachers in the fields of mineral technology have frequently complained that even in post-graduate groups there is an appalling indifference to their appeals for good English. Some have even noted a student's belief that the use of refined English is effeminate. If those with such immature beliefs could measure the pay-check damage arising from the use of "sloppy" language, they would realize that precision and refinement in English may be quite as important as technical accuracy. When the reader audience is without technical knowledge simplicity in treatment becomes especially important. If one is engaged in consulting work, in government service, or in any field where reports have public distribution, the language employed should be technically adequate but simple enough to be understood by non-technical readers. For example, one may use the term "visual" in place of "megascopic." Technical language can be so obscure that it cannot be understood even by highly-trained students. In the March-April (Vol. 47-No. 2) issue of Economic Geology, Nicholas Vanserg ridicules these extremes and quotes various paragraphs from published material, such for example: "However, lattice orientation unaccompanied by cognate dimensional orientation can never be attributable to growth from an isotropic blastetrix." "The temperature declines because of cessation of the exothermic chemical and mechanical equilibriopetal processes." These he calls "good geologese" and they are calculated not only to baffle the reader but to impress upon him the erudite character of the author. Revision In some cases, difficulty arises from the fact that the writer is too close to the subject and unconsciously assumes that his reader is equally familiar with the background of the report. It is difficult for the writer to regard his work objectively and to determine to what extent it is likely to be understood. Every important manuscript will gain in clarity if the author will have it reviewed by an informed reader. But the writer must not be oversensitive to criticism and should not treat his composition as perfect and beyond the possibility of improvement. The first draft of a report always requires revision, regardless of the care used or the ability of the writer. Three or four revisions are not uncommon. The first draft usually requires expansion in places, the deletion of non-essential material, and language changes to promote clarity of expression. This should be done by the author after a lapse of time, even if only overnight, in which his mind has been occupied on some other subject. Possible improvements are always more visible. The manuscript should be passed on to another reader for further suggestions. Organization of Material The engineer should study available reports and library references before going into the field. If the previous reports have been responsibly done and can be accepted as correct, then much field time can be saved. It is, of course, customary to make some on-the-ground checks to confirm earlier reports, particularly those relating to ore reserve which may have undergone changes. Report writing requires time and expense, but nevertheless, the basic reasons for conclusions should be presented even in the case of a worthless property, for it may prevent a duplication of the work. If the mine examined is obviously of no further interest, no useful purpose can be, served by preparing a report in detail. In one case an engineer travelled all the way to South America only to find that the mine had been grossly misrepresented and was valueless. His cabled report "Nonsense" is a case of over-simplification, but it served his company's purpose. The first step in report organization should be the selection of subjects. This should be done at the mine, and the data collected for each subject should be reviewed in considerable detail on the ground. Otherwise one may find that he has failed to collect some essential details not readily obtained after he has returned to headquarters. If the property to be described is undeveloped, then many of the subject titles are automatically eliminated. Usually no useful purpose is served by an attempt to calculate the cost of production under such circumstances, although the cost of exploration

Jan 1, 1952

By L. D. Hall, D. R. Mash

The paper presents the results of experiments on the anelastic. behavior of gold, as manifested by grain boundary relaxation. Two grain boundary internal friction peaks are found for 99.9998 pct Au. It is found that the peaks are associated with primary and secondary recrystallization. However, the existence of two discrete peaks cannot be explained on the basis of grain size and shape alone. It is suggested that grain boundary stability, as determined by orientation, plays a role in the observed effects. EVIDENCE for the viscous behavior of grain boundaries in metals has been presented in recent years by several investigators, based upon studies of various anelastic effects, especially internal friction. KG1 has contributed greatly to this field, having put forward a coherent body of evidence for stress relaxation by the viscous intercrystalline flow mechanism. In this connection, he has made extensive use of pure aluminum (99.991 pct) as the test material, although he has also studied other metals and alloys, including pure iron (Puron).² Rotherham, Smith, and Greenough³ have studied the internal friction of pure tin, interpreting their results in a manner similar to that of KG. In view of the importance of such studies in shedding light upon the fundamental structure and behavior of the grain boundaries in pure metals, it appears that the use of a very pure test material which is inert to its environment should provide useful information on anelastic properties and the source of such behavior in pure metals. The present work was carried out on spectrograph-ically pure, 99.9998 pct Au, free of all impurities except for a trace of silver, estimated to be present to the extent of about 0.0002 pct. The term "pure gold" will hereafter refer to this very pure material. Gold of commercial purity, 99.98 pct, was also studied to observe the effects of small amounts of impurities. A pure gold "single crystal" specimen was also tested for comparison. The variation of the internal friction and rigidity modulus as a function of temperature was determined by means of a torsion pendulum apparatus employing extremely low stress amplitudes and a frequency of vibration of the order of 1 cycle per sec. A 12 in. length of 0.031 in. (20 gage) gold wire formed the suspension element. The apparatus was similar to that described by Ke.l The test procedure and the basic requirements to be met for obtaining useful experimental data by this method have been given elsewhere.1,2 It should be made clear that in all of the experiments to be described, the internal friction and rigidity were independent of the amplitude of torsional vibration. The semilog plot of amplitude of vibration vs ordinal number of vibration was a straight line. This was carefully verified for each internal friction measurement. The linear variation shows that the internal friction was independent of stress; i.e., that the specimens were not being cold-worked during testing. The reproducibility of the internal friction curves, which were obtained by cyclic heating and cooling, indicates that the gold was unaffected by its environment during the tests. The measure of internal friction adopted in the present study is the conventional "logarithmic decrement," defined as follows: log. dec. = l/n In A0/An [I] where n is the number of cycles or vibrations; A,, the initial amplitude of vibration; and An, the amplitude after the nth cycle. When the logarithmic decrement is small, the shear modulus, G, of the wire is proportional to the square of the frequency of vibration provided the length and radius of the wire are kept constant. A plot of frequency squared vs temperature gives the following ratio:' This expresses the fraction of the stress which has not been relaxed at a given temperature. Gr and Gv are the relaxed and unrelaxed moduli, respectively. The frequency of vibration in the polycrys-talline specimen is fp, and the frequency of vibration of a single crystal is f8. This latter quantity is obtained simply by extrapolating the linear, low temperature portion of the curve of frequency squared vs temperature for the polycrystalline specimens. The theory of viscous grain boundary stress relaxation as demonstrated by the anelastic behavior of metals has been discussed in detail by Zener4 and need not be reproduced here. Experimental Results Initial measurements of the internal friction of pure gold were carried out on specimens which had been drawn with no intermediate annealing, resulting in a material which had undergone approximately 99 pct reduction of area in final processing. Annealing was then carried out at successively higher temperatures starting at 400°F for 1 hr and proceeding in this manner to as high as 1600°F in 100°F intervals. After each annealing treatment an internal friction and rigidity vs temperature curve was obtained over the range from room temperature to the particular annealing temperature. The resulting internal friction curves did not exhibit well defined maxima (peaks), but rather several fairly flat

Jan 1, 1954

By David C. Russell

The Department of the Interior used to be a quiet, noncontroversial, almost boring agency. It, after all is the fifth oldest of the Departments, and as an old line Federal agency it has studiously performed its preservation and resource management functions in a caretaker mode--though some would say more "undertaker" than "caretaker"--locking up the body and soul of America piece-by-piece. Yes, quiet, serene. That is until Jim Watt showed up. And we have all seen that version of Mt. Vesuvius which resulted--only it was the environmentalists who blew their tops. Ronald Reagan chose Jim Watt as Secretary of this fine old agency to prove that one-third of our Nation's land and over a billion acres on the Outer Continental Shelf can work for this Nation. At the foundation of President Reagan's charge to Secretary Watt is a belief in the tenets of the free enterprise system, and in the individual freedoms upon which this country was founded. There are those who don't share this belief in democracy and free enterprise, and those who believe this 205 year experiment called the United States of America will fail. Nikita Krushchev said "we will bury you"--obviously he didn't agree with our system. An Italian sociologist, Franco Ferrorotti, said bureaucratic stagnation will kill capitalism. Certainly we have all felt the ravages of bloated bureaucracies. Perhaps one indicator in the United States is the Federal Register, that daily compilation of Government's largesse. In 1970, 20,000 pages of the Federal Register were published. A decade later, in 1980, that volume had quadrupled to 80,000 pages. The Federal bureaucracy can stagnate from excessive budgets as well. The Interior Department spent $60 million on administering Federal coal leasing in 1981. That's nearly two bits a ton for every ton of coal leased in 1981. You wouldn't stay in business very long if your administrative overhead on inventory was that outrageous. But the pessimism of our critics is apparent from more than red tape and bloated budgets. For decades America has been fasting--consuming too little of America's wealth of minerals, subsisting instead on a diet heavily reliant upon mid-east oil, with little emphasis or concern for inventorying and developing domestic energy and mineral resources. Economics--yes. But short-term, short-sighted economics. Excessively dependent upon foreign imports, of oil, cobalt, chrome and other strategic minerals, the U.S. measures its time before another embargo--or fallen Shah, or Soviet manipulation, or Saudi shift, or, as we witnessed in Egypt, assassination--an untimely loss to mankind and efforts to bring peace to the troubled mid-east. These disruptions, in addition to their tragic human tolls, impair the free world's security. Huge chunks of the United States have been locked away in dozens of single land use categories in the name of conservation, with only the foggiest idea of what resources might be denied the American people-and this at a time of unacceptable levels of energy and strategic mineral imports. More than half and perhaps two-thirds of all Government-owned lands are totally withdrawn from or severely restricted to development under the mining and leasing laws. We must continue to rid Government of the overly zealous restraints which have been keeping us from drawing upon that which can help restore our economy and national security. When we assumed responsibility, the United States was dependent on foreign sources for about 40 percent of its oil. In 1981, our oil import bill was approximately $83 billion--nearly 17 times what it was in 1972. Our reliance on foreign sources for essential minerals is even more disturbing. We must look to other countries--some unfriendly, some unstable--for 22 of 36 strategically critical minerals. Yet the energy resources on federal lands which are owned by the American people could meet our needs for centuries if properly managed. Eighty-five percent of the crude oil yet to be discovered in America is likely to come from public lands, as will 40 percent of the natural gas, 35 percent of the coal, 80 percent of the oil shale, nearly all of the tar sands, and substantial portions of uranium and geothermal energy. Our vast hardrock-mineral wealth includes untapped deposits of essential elements we now import, such as chromium, copper, platinum, and cobalt. The obvious question is, if these abundant resources can help to revitalize our economic strength and to preserve our national security, why aren't we using them to better advantage? To a large extent, the answer can be found in past decisions to restrict public access to the federal estate, thus deferring to us or our successors the tough decisions that flow from Congress' mandate to provide for environmentally responsible development of America's energy and mineral treasures. Here is the legacy this Administration inherited: In January 1981, 7 years after the onset of the Mideast oil embargo: ---Less than 15 percent of federal onshore lands were under lease for oil and gas development; ---No oil and gas leases had been issued in Alaska for 15 years;

Jan 1, 1982