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By Michael Hoch, Walter C. Wyder

The Cr-Ni system was investigated between 900" and 1400°C and 45 to 100 wt pct Cr. The Cr-Fe system was studied between 1200" and 1385°C and 70 to 100 wt pct Cr. Powdered alloy compacts were produced from high-purity chromium, nickel, and iron poulders. The compacts were sintered in an argon atmosphere and then machined into small, 0.030-in. diam cylindrical specimens. These were then heated by induction in the high-temperature X-ray diJfractwn camem under a helium atmosphere and irradiated with copper Ka radiation. From the results of the high-temperature X-ray diffraction patterns it can be concluded that chromium exists only in the bcc form, and that no eutectoid reaction occurs in the Cr-Ni system in the temperature interval 900" to 1400°C. The X-ray diffraction patterns are in agreement with the Cr-Ni phase diagram of Bechtoldt and Vacher, and Williams. It is possible that chromium undergoes one or more allotropic transformations between room temperature and its melting point. Most of the evidence was gathered from the study of the chromium-rich ends of the Cr-Ni and Cr-Fe binary systems. All the investigations rely heavily on indirect methods: thermal analysis, electrical resistivity, and micro-graphic inspection of quenched samples. In the present work the chromium-rich side of the Cr-Ni and Cr-Fe binary systems is studied, using high-temperature X-ray diffraction techniques. Thus the coexistent structures can be observed directly at temperature. PREVIOUS INVESTIGATIONS ~ansenl shows two possible Cr-Ni phase diagrams 1) a simple eutectic [Liquid =a-Cr(bcc) + y-Ni(fcc)], 2) a eutectic [Liquid+ P-Cr(fcc) + y-Ni(fcc)] and euctectoid [p-Cr(fcc) ==a-Cr(bcc) + yNi(fcc)]. The latter is based on the work of Grant and co-workers.2 Stein and rant'" placed the eutectoid composition at 1215°C and 68 wt pct Cr; their diagram is shown in Fig. l. Similarly, Sully3 also discusses the two proposed diagrams. Price and Grant,4 working on an isothermal section of the Cr-Ni- Fe ternary diagram at 1300°C, made no mention of a ß-chromium phase (fcc). The ß-chromium structure was also reported by Misencik 5 in the Cr-Nb(Cb) system. Williams 6 studied the Cr-Ni system using precipitation techniques. His work included the chromium and nickel solvus lines below 1250°C. He reported no ß structure nor any eutectoid reaction. The solvus lines which he produced were very similar to those of Jette, et al 7 below 1000°C. He concluded that Grant and coworkers2 had misinterpreted their data, and that effects which they had reported were actually due to the rapid and extensive precipitation of the nickel-rich phase. Bechtoldt and vacher8 used sintered powdered alloy compacts in an attempt to find the ß phase. They used metallographic and room-temperature X-ray diffraction techniques and also failed to detect the fcc chromium phase. They attributed the low slope of the chromium solvus at approximately 1150°C as the probable cause of the abundant precipitation obtained. They also stated that the precipitation was the probable cause for the abrupt discontinuities in the thermal analysis and electrical resistivity data which led to the conclusion that a eutectoid reaction existed. Fig. 1 also shows their diagram. Grigor'ev and coworkers9 investigated the polymorphic changes of chromium in the Cr-Ni phase diagram. Using standard microstructural and thermal analysis techniques, they published a phase diagram which contained five polymorphic forms of pure chromium and four eutectoid reactions. They stated that the room-temperature bcc chromium transformed to a fcc structure at 930°C, to bcc at 1300°C, to hcp at 1650oC, and then finally to bcc at 1830°C. The eutectoid reactions were placed at 850°, 960o, 1140°, and 1220°C. Also to be noted was the fact that the uppermost phase, the bcc above 1830°C, was different from the upper phase of Grant and coworkers,2 the fcc above 1840°C. Their eutectoid reactions, temperatures and compositions fall

Jan 1, 1963

By Daniel R. Shawe

Large tabular beryllium deposits in waterlaid rhyolitic tuff at Spor Mountain, Utah, contain the world's largest known resources of beryllium (as bertrandite). The district also has produced fluorspar and uranium. The largest beryllium deposit is about 2.5 miles long, and known deposits contain many million tons of material with at least 0.5 per cent BeO. The beryllium-bearing tuff (Pliocene?) underlies topaz-bearing rhyolite ( Pliocene?) that contains unusually high amounts of beryllium, fluorine, and uranium, and overlies other volcanic rocks (Pliocene? or Micocene?) and marine carbonate and elastic rocks ( Paleozoic). The deposits occur in hydrothermally altered tuff only where it contains abundant carbonate pebbles eroded from the Paleozoic rocks and where the tuff was deposited as thick layers in now-buried paleovalleys. Basin and Range faults, thrust fa ults, and possibly strike-slip faults formed in this part of the Basin and Range province during the late Tertiary, and volcanic rocks were extruded. Beryllium mineralization probably occurred during this episode. Undoubtedly the beryllium deposits are related genetically to the topaz-bearing rhyolite, but the details of their genesis are not certain and probably are complex. Beryllium deposits are close to major faults, and locally the beryllium is concentrated at faults, indicating fault control of mineralization. Some elements in the deposits, such as lithium, however, are evenly distributed in certain Luff beds and perhaps were introduced prior to faulting. Still other elements, such as manganese and lead, were concentrated in the beryllium deposits and subsequently were leached along late fractures, indicating a period of metal redistribution following mineralization.

Jan 1, 1968

By John V. Beall

They let the whole world know again that not only could we do it, but we make it look easy. The great crews before Scott, Irwin and Worden of Apollo 15 have all blended warm humor, informality and dexterity to put on a good show: but it keeps getting better and the last one was the best. Scott's rendition of Galileo's experiment using a hammer and a feather--not just any feather, but a falcon feather after the name of the LEM-was priceless. One generation of school kids will never forget that lesson. The final touch was in the "would-you-believe''" category, Now if English astronauts had been performing the mission, the sign-off would have been typically low key. Something like; "well its tea time, chaps; we'll have to toddle along." Apollo 15 surprised and thrilled spectators by blasting off to the Air Force song "Off we go into the wild blue yonder" and leaving a camera behind to photograph their own ascent. Now that is what we call showmanship. There is another aspect to our space show and that is that it cost billions of dollars to put on. With that kind of backing, the world for an audience and in the face of grave personal risk, one would expect the space explorers to be all business. Instead they did their jobs with limpid buoyancy. Our older readers will recall and contrast a movie of the thirties and the tense atmosphere when they had to talk that kid up there (Franchot Tone) down through the zero ceiling. A feat of considerably less difficulty than docking LEM. but nevertheless the gut tightening drama was absent in the latter event. In another example, few of us can visualize reporting back after a business mission to one of the old barons such as J. P. Morgan in any but the most sedate and business-like terms. In fact we don't have to go that far back, as we can think of a few pepper-pot bosses we have had to whom one always played it straight.

Jan 1, 1971

By P. W. Barton, A. A. Johnson, E. J. Hughes

THE only systematic work on the effect of carbon on the recovery and recrystallization kinetics of iron so far reported in the literature is that of Venturello et al.1 These workers found that doping high-purity iron so that it contained up to 86 ppm C caused a marked retardation of recovery but had little or no effect on the recrystallization kinetics. Such evidence for an effect as was obtained was inconclusive. In the course of a study of electron-beam zone-refined iron the authors have recently examined the effect of added carbon on the recrystallization kinetics of this material. The amount of carbon added was about 50 pct more than was used by Venturello et 01. and definite evidence was obtained that carbon at this level retards recrystallization. The starting material was taken from a batch of 0.2-in.-diameter Johnson-Matthey spectroscopically pure iron rods which had been further purified by being given three passes at 4 in. hr-1 in a standard MRC electron-beam zone-refining unit. The purity of this material. which was used in two other investigations of the properties of high-purity iron,2,3 was established by an extensive series of analyses. Four laboratories, the National Research Corp., Newton, Mass., the Naval Research Laboratory, Washington, D.C.. the Battelle Memorial Institute, Columbus, Ohio, and the National Physical Laboratory. Teddington. Middlesex, England. carried out analyses for carbon. oxygen. and nitrogen. and in addition a complete mass-spectrograph analysis was carried out at Battelle. In all, twelve analyses were carried out for carbon, seventeen for oxygen and twelve for nitrogen. The amounts of these elements found to be present were 10 * 7, 8 i 5, and 0.9 i 0.1 ppm, respectively. The limits given are rms deviations. Two results, one of 46 ppm of oxygen and another of 31 ppm of nitrogen, were rejected as anomalous. The mass-spectrograph analysis revealed the major impurity to be 25 ppm of tungsten. All of the other elements detected were present in amounts less than 0.5 ppm. Some of the rods were doped with carbon by being immersed in a suspension of carbon in oil, heated in a vacuum at 400°C, and then zone-leveled to make the distribution of carbon uniform. Carbon analyses carried out on three of the doped rods gave a mean value of 130 ± 45 ppm. Some of the doped and undoped rods were deformed 58 pct by swaging and cut into specimens 1/2 in. in length. Isothermal recrystallization experiments were then carried out on them at 575", 600°, 615", 630°, and 650°C, the volume fraction of each specimen recrystallized being measured by a point-counting method described by Hilliard and Cahn.4 The results for the two types of specimens are shown separately in Figs. 1 and 2. In Fig. 3 the pairs of recrystallization curves for each temper-

Jan 1, 1965

By D. Geiselman, A. G. Guy

Single cvystals were grown from high-purity magnesium containing known amounts of nitvogen in the range 0.0008 to 0.0048 wt pet. Crystals of known ovientation were tested in tension in an Instron ma chine to determine the yield strength and to obsevue wheather a yield point occurred. Slowly cooled crystals or those given a solution heat treatment did not show a yield point. However, crystals that were aged following a solution treatment showed a yield point for all of the nitrogen contents studied. It was concluded that nitrogen caused the yield point by the Cottrell mechanism. NITROGEN has been shown to produce sharp yield points in single crystals of cadmium, zinc,2'3 ß-brass,4 and iron,5,6 as well as in polycrystalline iron7 and molybdenum.8,9 Since magnesium has a structure similar to zinc and cadmium, it seemed reasonable that magnesium should also exhibit a sharp yield point provided it contained sufficient nitrogen. Bobalek and Shrader10 reported a total nitrogen content of 0.002 to 0.0065 wt pct in com- mercial magnesium alloys, an amount well in excess of that required by theory. However. magnesium differs from cadmium and zinc in that it forms a stable nitride, Mg3N2, which has a standard free energy of formation of -95,480 cal per mole at 25" c." If rather than being in solid solution, the nitrogen were predominantly combined as the nitride, it could not act to produce a yield point. This type of behavior is the basis for the elimination of strain aging and a yield point in steel by the addition of strong nitride formers such as titanium,12 columbium,13 aluminum,14 vanadium,15 and boron.16,17 Thus, there appeared to be factors both favorable and unfavorable to the production by nitrogen of a sharp yield point in magnesium, and the purpose of this investigation was to determine the actual behavior of magnesium crystals containing known amounts of nitrogen.

Jan 1, 1960

By H. Margolin, A. Coucoulas

Fused alumina or silica crucibles were used as the containing vessel. X-ray powder photographs were taken with CrKcll radiation and the use of Straumanis type Norelco cameras of 114.6 mm diam. Crystallographic data for these compounds are shown in Table I. These results are in agreement with others of this series reported previousiy by Wernick and Geller.l The abnormally large atomic volume of Eu and Yb metal3 is manifested in EuAl2, and YbAl2, when one compares them with the compounds reported in Ref. 1. However, the behavior of Yb in the Ni compound is the same as that observed in Ni5Yb having the Cu5Ca structure.4 Thus, it appears that Yb has a valence closer to 3 only in the Ni compounds; i.e.. the 2s and Id electrons are lost to the conduction band.1,4 Europium in EuAl2 appears to have a valence closer to 2. In previous work.' X-ray patterns of ingots of NdCo2 indicated a multiphase material with faint indication of the presence of a phase having the MgCu2 structure. It was thought that NdCo2 formed peri-tectically from the melt, resulting in a multiphase system when cooled under nonequilibrium conditions. An X-ray pattern of a sample from a melt cooled more slowly than in past work showed that the major phase was NdCo2. The lattice constant, Table 1, is in excellent agreement with the value one can predict from the data of Ref. 1. One of the other phases was identified as Co5Nd. The author wishes to thank J. H. Wernick for his guidance in this work, and D. Dorsi for the preparation of these compounds. 'J. H. Wernick and S. Geller: AIME Trans., in press. 'J. H. Wernick and S. E. Haszko: to be published. 'F. H. Spedding and A. II. Daane: Progress in Nuclear Energy, Series 5, Eds.: H. M. Finniston and J. P. Howe, McGraw-Hill Book Co., 1956. 'S. E. Haszko: to be published. 'J. H. Wernick and S. Geller: unpublished work. 6J. 11. Wernick and S. Geller: Acia Cryst., 1959, vol. 12, p. '162. A reinvestigation of the lattice parameters of Ti-Sn alloys by the present authors has revealed consistently hiher c and a values than those obtained by Worrier. The difference is most pronounced in the c-parameters which are, therefore, used as a basis of comparison. This discrepancy was not due to air contamination, since precautions were taken to exclude this possibility. Specimens for Debye-Scherrer photograms were prepared by arc-melting 15-g buttons of Bureau of Mines titanium and 99.99 pct Sn, with compositions of 6, 8, 10, and 12 at. pct Sn. These buttons were forged under an oxygen-acetylene torch to 1/8-in. sq rods to produce relatively fine grained material. Scale and some surface were ground off, and the rods, after wrapping in molybdenum and titanium sheet, were vacuum annealed 15 min at 800 °C to remove hydrogen. Heat treatment of one of the samples at 875°C to produce ß and reveal a at the surface showed no surface contamination. Following the vacuum treatment, the specimens were wrapped in molybdenum and annealed for 1 week at 800°C under two atmospheres of argon. After water-quenching, the rods were ground so that the thickness tapered to 0.1 mm at the tips. The ground specimens were then recapsuled as previously and reannealed 1 hr at 800°C to remove cold work. The

Jan 1, 1961

By Paul M. Tyler

Higher freight rates and better methods of beneficiation now may make it more economical to open inferior deposits closer to a glass factory than to work higher-grade deposits farther away. Nature of impurities and special treatments as well as common practice of sulphuric acid leaching are described. HISTORICAL concepts of the economics of the glass-sand industry are changing rapidly. The greatly expanded demand for glass containers combined with higher freight rates on raw materials and manufactured products have induced a migration of glass factories toward densely populated centers and the creation of new standards of place value for substandard sand deposits. This migration has been facilitated by the construction of pipelines to bring cheaper natural gas and liquid fuel to large cities and may be further speeded by the adoption of modern mineral dressing methods to permit economical utilization of local raw materials. Our national resources of naturally high-grade silica sand are abundant, but most of the best deposits are situated so far from large centers of population that it now costs $3.00 to $5.00 a ton to carry the sand from the mine to the optimum site for a factory making beverage bottles, scientific and electrical glassware, and miscellaneous blown and pressed ware for local markets. It follows that on the basis of freight savings alone it may be economical to use material from inferior deposits closer to the factory even though the f.O.b. cost of mining and treatment may be much higher than at a higher grade deposit farther away. Particle-size distribution is a feature of glass-sand specifications. As long as glassmakers insisted upon having their sand principally coarser than 100-mesh, any material was automatically excluded from consideration that could not be purified without fine grinding or other drastic treatment which greatly reduces the size of the quartz grains. However, re- cent large-scale tests in Norway' showed that finely-crushed quartz used in a soda-lime-silica glass batch caused it to melt and become refined appreciably faster than when ordinary coarse (Belgian) sand was employed. Dust losses were negligible. Since the pre-war cost of sand was only 3 pct of the manufacturing cost of the glass, it was deemed economical to pay twice as much for crushed quartz because of the saving in wear and tear on the furnace walls. In the author's unverified opinion, sand ranging in size between 150 and 400-mesh would probably be superior to that in the more usual range of 20 to 100-mesh. Former objections to fine sand (other than dust) were doubtless fostered by the natural concentration of impurities in the finer sizes. Ordinarily the most objectionable, as well as the commonest, impurity from the standpoint of the manufacturer of any but the cheaper qualities of colored glass is iron. No natural sands are really pure silica. Even water-clear quartz crystals are likely to contain impurities in the form of solid solution as well as inclusions which cannot be eliminated except by chemical treatment that will break down the silica lattice. Pure white pegmatite quartz will usually analyze 0.01 pct or more of iron oxide, and ordinary vein quartz and the quartz grains in most

Jan 1, 1951

By Paul M. Tyler

Higher freight rates and better methods of beneficiation now may make it more economical to open inferior deposits closer to a glass factory than to work higher-grade deposits farther away. Nature of impurities and special treatments as well as common practice of sulphuric acid leaching are described. HISTORICAL concepts of the economics of the glass-sand industry are changing rapidly. The greatly expanded demand for glass containers combined with higher freight rates on raw materials and manufactured products have induced a migration of glass factories toward densely populated centers and the creation of new standards of place value for substandard sand deposits. This migration has been facilitated by the construction of pipelines to bring cheaper natural gas and liquid fuel to large cities and may be further speeded by the adoption of modern mineral dressing methods to permit economical utilization of local raw materials. Our national resources of naturally high-grade silica sand are abundant, but most of the best deposits are situated so far from large centers of population that it now costs $3.00 to $5.00 a ton to carry the sand from the mine to the optimum site for a factory making beverage bottles, scientific and electrical glassware, and miscellaneous blown and pressed ware for local markets. It follows that on the basis of freight savings alone it may be economical to use material from inferior deposits closer to the factory even though the f.O.b. cost of mining and treatment may be much higher than at a higher grade deposit farther away. Particle-size distribution is a feature of glass-sand specifications. As long as glassmakers insisted upon having their sand principally coarser than 100-mesh, any material was automatically excluded from consideration that could not be purified without fine grinding or other drastic treatment which greatly reduces the size of the quartz grains. However, re- cent large-scale tests in Norway' showed that finely-crushed quartz used in a soda-lime-silica glass batch caused it to melt and become refined appreciably faster than when ordinary coarse (Belgian) sand was employed. Dust losses were negligible. Since the pre-war cost of sand was only 3 pct of the manufacturing cost of the glass, it was deemed economical to pay twice as much for crushed quartz because of the saving in wear and tear on the furnace walls. In the author's unverified opinion, sand ranging in size between 150 and 400-mesh would probably be superior to that in the more usual range of 20 to 100-mesh. Former objections to fine sand (other than dust) were doubtless fostered by the natural concentration of impurities in the finer sizes. Ordinarily the most objectionable, as well as the commonest, impurity from the standpoint of the manufacturer of any but the cheaper qualities of colored glass is iron. No natural sands are really pure silica. Even water-clear quartz crystals are likely to contain impurities in the form of solid solution as well as inclusions which cannot be eliminated except by chemical treatment that will break down the silica lattice. Pure white pegmatite quartz will usually analyze 0.01 pct or more of iron oxide, and ordinary vein quartz and the quartz grains in most

Jan 1, 1951

By W. M. Peirce, E. A. Anderson

A FEW metals have been known since the dawn of history. Many have been prepared in quantity only within the present century. Zinc falls into an intermediate category, although there is some evidence of its existence in elemental form in Greece as early as the third or fourth century B.C. Nevertheless, the first important use of zinc antedates the earliest records of civilization. This first use was in the alloy, brass, which is roughly one third zinc. This continues to the present time as one of the major uses of the metal. The first production of brass, in light of present knowledge, was perhaps one of the 'most romantic and fortuitous of technical discoveries. Copper, the major constituent of brass, had been given to man by Nature in the native state; that is, as lumps of fairly pure copper. The art of melting and working it had been learned. But zinc does not occur as the metal in Nature and even if some early metallurgist happened to heat zinc ore with a reducing agent, the reduced metallic zinc passed off as vapor and was lost. Doubtless some early coppersmith, melting copper in accidental contact with zinc ore, reduced the zinc, and the vapor was absorbed by the molten copper. Its color, hardness, and other properties were thus wonder- fully changed. And so the earliest metallic form of zinc, as nearly as we can deduce, existed in the alloy brass. Probably knowledge of the kind of rock with which to heat copper to change it to brass, the best

Jan 1, 1953

By Edmund J. Pryor

DURING the war years restrictions on travel, pressure of work, and the irregular arrival of technical literature from abroad combined to severely isolate Great Britain in a period of intense war expansion of the art and practice of mineral dressing. Many British technicians were fully occupied with the day-to-day problems of improvising substitutes as regular sources of supply failed. and with mastering the strange demands and working conditions of wartime. After a long day spent between ones laboratory and production work, the rest of the waking hours were often filled with fire watching or home guard patrol activities, substituting for a night-shift manager, or "resting" in a dugout while the bombs came down. There was no time for serious study of such technical literature as survived the Atlantic crossing.

Jan 1, 1947

By S. Zador, C. B. Alcock, K. Sudo

Measurements have been made of the standard free enevgies of formation of the sulfates of cobalt, Cupric copper, nickel, and ferric iron in the temperature range of 750° to 950°C. Dynamic gas-solid techniques have been employed in which oxide-sulfate and basic sulfate mixtures were placed in a stream of gas of controlled SO3 potentials. Thermal analysis and thermogvavimetry were used as detection methods, and it was found THE formation of sulfates during the roasting of sulfide ores is now considered to arise in many cases from the interaction of sulfur trioxide in the gas and the metal oxide which is formed on the sulfide as a first step.' As a preliminary to the investigation of the kinetics of sulfate formation during roasting, measurements have been made of equilibria from which the free energies of formation of cobalt, copper, nickel, and iron sulfates can be that the range of temperatures which could be investigated and the choice of method was largely controlled by the kinetics of these gas-solid reactions. The results are compared with previous results obtained from static measurements with which they agree quite well, and calculations have been made employing themal data to interrelate the present results with those for other sulfates. calculated. The method used has been to expose the solid sulfate (or basic sulfate) to a controlled flowing gas mixture of SO,, 02, and SOs and to observe the temperature of decomposition. The onset of decomposition was detected by thermal analysis or thermogravimetry. EXPERIMENTAL METHODS The thermal-analysis method was similar to that employed by Dewing and Richardson.' The sulfate was dehydrated at 250°C in air, and placed in a small alumina crucible which was held by a quartz ring in the hot zone of a horizontal furnace. The reaction tube of this furnace was made of mullite.

Jan 1, 1965

By David A. Summers, John Corwine, Li-King Chen

The results from fracturing plexiglas beams are combined in eight existing equations to determine the surface energy of the material. The reliability of each equation is tested, and the equation in use to determine fracture toughness is found to be the most exact. This equation is then used in determination of the surface energy of Barre Granite.

Jan 1, 1971

By G. E. Keller

In connection with the work of Committee D5, Coal and Coke, of the American Society for Testing and Materials in developing new standards and improving old standards, series of tests were made to check the variance of sample preparation and analysis of American coals. Table I in the "Tentative Method of Preparing Coal Samples for Analysis - 02013-62T" is rather complicated, and the tests were designed to develop data for the simplification of this table. An allowance of 20% of the total variance of sampling and analysis for the sample preparation and analysis steps was used. Also, instead of coals being grouped into ash ranges, they were grouped as washed and raw (unwashed) coals. As a result of these tests, a simplified Table I for Tentative Standard 02013 has been proposed. A standard test for laboratories to check their variance of sample preparation and analysis has been developed. Committee D5 on Coal and Coke of the American Society for Testing and Materials has been making a study of all standards applying to coal for the purpose of improving and bringing them up to date and for breaking some of the existing standards covering a number of tests into single standards. As an illustration, sample preparation is now partly covered in ASTM Designation D492-48, Sampling Coals Classified According to Ash Content, and partly in ASTM Designation D271-58, Laboratory Sampling and Analysis of Coal and Coke. The latter contains, in addition to parts of sample preparation, methods for determining Moisture, Ash, Volatile Matter, etc. Although revision of sampling methods and sample preparation methods are now assigned separately, it is possible that they may end up as one standard. One of the first new Tentative Standards developed as the result of these studies was ASTM Designation D2013, Tentative Method of Preparing Coal Samples for Analysis. Although this method is quite an im- provement over that in the old standards and gives very specific instructions, Table I (attached) is quite complicated and rather hard to understand. In order to take advantage of reduced quantities or weights, it is necessary to know the ash content within rather narrow limits before sample preparation and no distinction is made as to whether the coal is cleaned or uncleaned. No limits of accuracy are assigned to the sample preparation and analysis. The total over-all accuracy of sampling, preparation and ash determination as given in D492-48 has been specified for commercial sampling procedure as follows: "This procedure is intended for an accuracy such that if a large number of samples were taken from a single lot of coal, the test results in 95 out of 100 cases would fall within ? 10 per cent of the average ash content of the sample." Although Appendix 11, Method for Determining the Over-All Variance of Reduction and Analysis in the Tentative Methods for Mechanical Sampling of Coal, ASTM Designation D2234-63T, does give a method for determing the over-all accuracy of preparation and analysis expressed as variance and also the F test, it does not permit the determination of the variance at the various stages of reduction or of the ash determination. It was decided in 1961 to ask a number of laboratories to run a series of tests for the purpose of determining the variance at various stages of reduction and analysis with the view of simplifying Table I of the Tentative Standard D2013-62-T. This paper is a record of this series of tests with recommendations which resulted from the tests. At the same time and preceding these tests the International Organization for Standardization under Committee TC/27 WG 7 was studying the same problem. Tomlinson1 of England and Dr. paul2 of West Germany had made studies giving quite a bit of information. Also Schwerd and coryel13 published some information which was the main basis for the Mechanical Division provision in ASTM Tentative Standard D2013-62T, Table I. In checking with the various laboratories which offered to cooperate in these tests, none was found which used mechanical division through the entire preparation procedure. It was then decided to use riffles at all stages with the thought that if riffles gave satisfactory variances, approved mechanical

Jan 1, 1965

By Charles Rich, Robert Munson, Leonard Obert

Improved methods of predicting the caving characteristics of ore bodies is discussed. Experiments were conducted at Climax mine, Climax, Colo., on varied rock compositions. The cavability of adjacent areas, as well as seismic energy absorption proved to be good factors in determining cavability. Seismic velocity, core recovery, and rock quality designation (RQD) were found to be not as reliable.

Jan 1, 1977

By J. Gordon Parr, D. H. Polonis

The formation and subsequent decomposition of metastable phases in Ti-Ni alloys containing up to 11 pet (atomic) Ni have been studied. The decomposition of a completely retained ß phase and of a completely transformed 8 phase in a 6 pet alloy has been followed by X-ray diffraction and metallographic methods and by hardness determinations made during the process. The possible mechanisms of the reactions are discussed. PREVIOUS investigations of the Ti-Ni system have usually been limited to phase diagram studies; but little attention has been given to metastable phases and tempering processes. These are important, however, since equilibrium conditions are rarely achieved—nor, perhaps, are they desired—in practice. Up to the present time the available transformation data for titanium alloys appear to be restricted to isothermal transformation curves for selected binary and ternary systems. No quantitative studies have been made of the mechanism by which equilibrium is approached. Several independent investigations have been carried out to determine the Ti-Ni phase diagram. Early work by Wallbaum' and later by Long et al.' produced tentative phase diagrams which were not representative of true binary conditions, since the alloys were contaminated with oxygen and nitrogen. The most recent diagram (Fig. 1) is due to Margolin et al.," and a slight modification of the a + ß/ß boundary (shown dotted) has been proposed by McQuillan.' The structure of the phase Ti,Ni was shown by Duwez and Taylor" to be face-centered-cubic, with 96 atoms per structure cell. The formation of a martensitic ß phase (close-packed-hexagonal) in Ti-Ni alloys has generally been observed when specimens of low nickel content are rapidly cooled from the 0 (body-centered-cubic) range. Margolin et al. reported an increasing tendency for P to be retained in lump specimens as the nickel content increases. McQuillan' has studied the effect on the microstructure of delay time in quenching, and has reported the formation of pro- eutectoid a precipitate in a quenched hypoeutectoid alloy. In a previous study of Ti-Fe alloys," experiments were made on powder specimens produced by filing alloy ingots. Techniques were devised for the preparation and heat treatment of alloys, and X-ray diffraction methods were used both for structure determinations and phase ratio estimations. A similar approach has been made in this study of Ti-Ni alloys. Experimental Methods Ten alloys ranging from 0.25 pet to 18 pet Ni* * All compositions are in atomic percentages unless otherwise stated. were prepared from iodide titanium bar stock (hardness Rf 72) and Johnson-Matthey spectrographic standard nickel by levitation melting.' As a check

Jan 1, 1957

By E. H. Lancaster, M. E. Mitchell

A MUD-conditioning program found to be very effective for drilling and completion operations on routine field wells requiring relatively short drilling time involves a moderate alkaline-tannate-bentonite treatment resulting in an ultimate filtration rate of 10.0 cc or less (API test). Mud weight schedules are planned from pressure information on completed wells in producing reservoirs and drill-stem test data obtained on other zones not being produced at present. In general, terminal mud viscosities average 45 sec (Marsh). This value has been found to be sufficient to remove cuttings from the well bore on the average well, with the slush pumps in general use on the rigs. On field wells requiring drilling times in excess of approximately 30 days, an alkaline-tannate-lime-bentonite treatment has been effective in maintaining desirable viscosities and filtration rates with a substantial reduction in chemical costs. This system has shown particular advantage on heavily weighted muds and those with abnormal flow-line temperatures. For the most part, the chemical treatment utilized in wildcat drilling follows closely the program used on field wells, depending on depth and duration of drilling operations. Wildcat mud programs are planned from information available from various geologic and operational sources, taking into consideration the possibility of encountering mud problems of a special nature in the wildcat area. Careful planning of wildcat mud pro- grams has proved to have definite value in avoiding most serious mud problems. An analysis and recommended treatment are presented on several special. mud problems which have been encountered in the area in the past. Those problems discussed are lost circulation, blowouts, sloughing shale, excessive chloride contamination, sulphate contamination, and prevention and correction of cement contamination. Introduction Drilling-mud control in the Southwest Texas area, in general, does not involve the multiplicity of problems encountered in other coastal areas. For instance, it is rare that a mixture of problems such as lost circulation, abnormal pressure, severe sloughing shale, and others, occurs on one well within close enough limits in vertical depth not to be taken care of by a sensible casing program, together with a relatively clear-cut mud program. There are conditions such as the fairly widespread occurrence of abnormal pressure in the lower Frio and Vicksburg zones, and the tendency for sloughing shale in the Jackson section which make for rather expensive mud control. However, the availability of fairly accurate geologic and operational information makes possible a reasonable degree of standardization on mud treatment over a relatively large area. It may be said that, over most of this area where drilling is currently in progress, the natural mud made is very poor in quality, but responds readily to moderate chemical treatment to yield very good wall-building characteristics. AS far as field development drilling is concerned, the mud engineer's principal job, once the routine treatment best

Jan 1, 1949

By J. W. Leonard, B. A. Donahue

A method is described for incorporating coal petrography into mining and preparation plant quality control based on conventional analyses. Complete analyses are made of each of the uniform and relatively distinct petrographic bands in a coal face. With this information it is possible to develop petrographic standardization curves. These curves permit diverse coal characteristics to be rapidly monitored by application of a few standard coal tests. Single seam quality control is discussed in this paper. Inquiries continue to be made about coal petrography, and specifically, about whether coal petrography should be applied more extensively in the coal industry. Coal petrography is the study of the distinct physical, optical, and chemical increments which make up the organic rock mixture which we know as coal. Petrography can be applied by any coal company or at any coal mine where conventional coal analytical facilities are available and where additional resources can be allocated for an increased number of determinations. This first paper of a two part series includes (1) a proposed conventional approach to single seam petrography based on the development of petrographic standardization graphs and (2) some informative and supplemental interrelationships involving coal characteristics developed as a result of this research. In the second part of this series, to be published at a later date, those petrographic characteristics of bands taken from many different coal seams located over wide geographic areas which can be closely related to each other will be considered. These findings will be examined looking toward the development of a comprehensive, conventional approach to coal petrography which can be used as a common basis for multi-rank petrographic standardization graphs. Implicit to the understanding of coal petrography is the well established fact1,2 that the individual analyses of distinct petrographic bands often differ widely from the average analysis which is used to characterize a whole coal seam. In fact, a distinct and minor banded increment of coal in a high volatile seam may actually be a medium or low volatile coal with an analysis similar to the average analyses of seams located in distant coal fields. During the mining of coal, much degradation is caused which tends to randomly scatter coal bands. The degraded, scattered, and physically separated constituents of distinct petrographic bands are processed side by side in the coal preparation plant as distinct petrographic fractions with particles grouped according to a narrow size range (which derives in part from common hardness), specific gravity, and-or surface chemistry. Tile data obtained from numerous analyses made on each of the bands of any given coal seam, although diverse, can be readily interrelated. Indeed, these interrelationships can be developed into a series of nomographs or petrographic standardization graphs to serve as a basis for developing a conventional petrographic* program. Thus, by analyzing one property (for example, ash) of a selected petrographic fraction collected or separated from the flow of coal in a preparation plant, it should be possible to estimate the other physical, chemical, and thermal properties of this fraction by referring to the petrographic standardization graphs. It follows that any or all petrographic fractions in the total coal flow originating from a single coal seam can be rapidly monitored for many properties on the basis of a single analysis run on each fraction. In recent years coal petrographic research has concentrated heavily on that phase of this work which involves microscopic reflectance measurements made at many minute and selected points on a coal briquette surface.3,4 Thus, the percentage of the total number of reflectance measurements that fall into each of a consecutive series of arbitrarily chosen reflectance classes are used to characterize coal. This procedure is analagous to using the face of a coal briquette to represent the reflectance characteristics present at the face of a coal seam. Moreover, by analyzing petrographic fractions of known and uniform optical properties it is possible to closely relate reflectance to other coal characteristics. For example, reflectance has long been known to be related to such

Jan 1, 1968

By Ernest R. Dickie

BRIEFLY, the ore body of the Bagdad Copper Corp., Bagdad, Ariz., is a monzonite porphyry carrying copper values fairly evenly distributed from the surface down through the primary zone. Tabular in shape, the ore body extends over several hundred acres. The oxidized zone averages about 60 ft thick and assays about 0.50 per cent copper. Under this is the chalcocite zone, or the zone of secondary enrichment, which averages about 100 ft in thickness and assays about 1.4 per cent copper. Under this zone lies the primary zone which extends in places to a known depth of about 150 ft and averages in grade about 0.60 per cent copper. Several years ago the block-caving method of extracting the ore from the chalcocite zone was installed. Then it was necessary to draw only about 250 to 300 tons per day, the capacity of the old milling plant. Early in 1943 the new 2500-ton concentrator was put into production. Drawing ore from the developed stopes in sufficient tonnage to furnish the mill at capacity proved unsuccessful in more ways than one. First, drawing the ore at an accelerated rate caused a large amount of dilution, there-by lowering the grade, and also caused funneling through to the surface. The surface material was detrimental to milling metallurgy and development of these stopes was costly per ton of ore extracted. The grade of ore decreased. making it impossible to maintain a mill head of over 0.9 per cent copper. The

Jan 1, 1947

A High-speed Dilatometer and the Transformational Behavior of Six Steels in Cooling. By Arthur L. Christenson, Edward C. Nelson and Clarence E. Jackson. (With discussion).................................606 Dilatometric Studies of the Graphitization of Cast Iron. By N. A. Ziegler. With discussion) 627 An Interferometer Type of Dilatometer and Some Typical Results. By- L. '4. WIlley and W. L. Fink. (With discussion).........................642 The meeting was held in the Pine Room of the Statler Hotel, Cleveland, Ohio, on Tuesday afternoon, October 17, 1944. The chairmen were F. M. Walters, Jr. and Howard Scott. Introduction F. M. Walters, Jr.—The principal advantages of the dilatometric method perhaps are two, as compared with the method of thermal analysis. One is that the dilatometric method can be applied with a large variety of rates of heating and cooling, whereas thermal analysis—that is, the study of the transformational characteristics by means of heat evolution—is limited to the rates of heating and cooling that reveal the evolution of heat. The dilatometer can be used for the study Of reactions at zero rates of heating and cooling; that is, isothermal reactions. As you will hear this afternoon, the rates have been pushed up as far as 500°C. a second. The other advantage is that the dilatometric method shows that a two-phase region is a two-phase region, whereas the thermal analysis merely reveals the temperature at which the rates of heat evolution are greatest.

Jan 1, 1945

By G. G. Hancock, H. H. Johnson

Hydrogen gas at atmospheric pressure is shown to cause substantial embrittlement in a martettsitic high-stretzgth steel. Subcritical crack growth is observed at very lom stresses and with high growth rates. It is suggested that an adsorbed layer of hydrogen atoms at the crack-tip surface provides the damaging hydrogen. Oxygen in small quantity, as little as O.7 pct by volume, is shown to eliminate subcritical crack growth in gas environments caused by hydrogen or water vapor. However, dissolved oxygen in water has little or no influence upon crack-growth rates. Oxygen-stopped cracks may be restarted by water, or by hydvogen or water vapor if oxygen is removed from the environment. These observations are interpreted in terms of preferential adsorption of oxygen at the crack tip and the formation of an oxide barrier. RECENT investigations1-3 have demonstrated that environmental factors are frequently responsible for delayed failure in martensitic high-strength steels. The environment causes crack initiation from preexisting cracklike flaws at unexpectedly low stresses, often far below the uniaxial yield strength. The crack then propagates at a rate controlled by the environment and the crack-tip stress-field intensity; during this period crack propagation will cease if either the stress or the aggressive environment is removed, and this may be considered a definition of subcritical crack growth. Fracture occurs when the crack has grown to a critical length, such that the fracture toughness of the steel is exceeded. Several liquids are known to cause delayed failure, but water and water vapor are the most severely damaging of the environments investigated to date.'-3 It has been suggested that hydrogen produced during corrosion reactions may be the actual embrittling agent2 The severe embrittlement caused by water vapor inevitably raises the question as to whether other gas environments are damaging. Previous work4'5 has demonstrated that high-pressure hydrogen (2250 psi or greater) is an effective embrittling medium, as measured by such criteria as reduction in area, notch tensile strength, and time to failure. Moreover, the embrittlement was eliminated by the addition of small quantities of air or oxygen to the high-pressure hydrogen, but it was not influenced by additions of nitrogen or argon.4 In the present study attention is focused upon gas environments at atmospheric pressure, in particular hydrogen and oxygen. The influence of these constituents upon the initiation and growth of a crack from a pre-existing cracklike flaw in a high-strength steel was determined directly by the electric-potential method of monitoring crack growth. MATERIALS AND PROCEDURE The H-11 steel was supplied by the U.S. Naval Research Laboratory as 3 by 12 by 0.065 in. sheet specimens with 1-in. transverse center slots. The slot tips were finished by Elox machining to a radius of 0.001 in. or less. The yield strength was 230,000 psi; chemical composition and heat-treatment schedule are given in Table I. The experimental apparatus, precracking procedure, and incremental loading sequence have been described previously.3 In the only significant change, precracking was sometimes carried out by a hydrogen embrittlement and baking technique. All experiments were conducted at room temperature; the hydrogen gas environment was purified by a commercial palladium purifier. Crack initiation and propagation were followed by the electric-potential method,'-3 using a calibration that has been recently dicussed. Stress-field intensities at the crack tip were computed by the conventional Irwin frmula; the plasticity correction was negligible and therefore not included. EXPERIMENTAL RESULTS A striking brittleness associated with molecular hydrogen at atmospheric pressure is demonstrated by the data in Table I1 and Fig. 1, which indicate that subcritical cracks in hydrogen initiate at lower stress-field intensities and propagate more rapidly than in fully humid argon. Ki and Kf are the crack-tip stress-field intensities at initiation and termination of subcritical crack growth, respectively. Termination, of course, corresponds to fracture. In both hydrogen and humid argon Ki is less than Kf

Jan 1, 1967