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By John Dasher, M. C. Chang

The Crucible mine in Pennsylvania, operating on Pittsburgh seam coal, is rated at 5000 tpd. The washing plant, built in 1943, is rated at about 400 tph, using hydroseparator boxes to wash the coarse coal (4 x 5/16 in.) and hydrotator units for the fine coal (5/16 x 0). It is generally acknowledged that gravity concentration equipment cannot be used efficiently to beneficiate coal finer than about 65 mesh. Before the present flotation circuit was installed, Crucible recovered its fine coal slurry, predominantly -24 mesh material, by passing it through a battery of five 14-in. and one hundred and ten 3-in. Hey1 & Patterson cyclones in parallel with a 75-ft Dorr thickener. About two thirds went to the cyclones and one third to the thickener. Underflows from cyclones and thickener were filtered, respectively, in one 12-disk Eimco and two 4-disk Oliver filters fitted with stainless steel cloth. The resulting cakes were added to the coarse metallurgical coal. The filtrates, overflow from the 3-in. cyclones, and thickener overflow were recycled to the coarse coal plant.

Jan 3, 1959

By E. F. Thomas

THE late George S. Rice was active in the inves--I- tigation of bumps, particularly in the last ten years of his career as chief mining engineer of the U. S. Bureau of Mines. Since most of his investigation was carried out in Great Britain, continental Europe, and—to a lesser extent—Canada, his thinking on prevention was influenced considerably by the experience of those countries. It is not surprising, therefore, that when he was called upon a few years before his retirement to investigate bumps in the U. S. and suggest ways to prevent them, he turned to longwall mining. A longwall method had been most successful in combating the bump hazard in mining coal under deep cover, especially in Great Britain, but the prevailing method there at the time was advancing longwall mining, which he knew was uneconomical under U. S. mining conditions. For this reason he proposed a modified retreating longwall system that he believed included the best features of the advancing method. As brought out by Rice,' if the cover is 2000 ft and 50 pct of the coal is extracted, the static load on the remaining pillars will be about 4000 psi, which exceeds the ultimate crushing strength in most instances. If the pillar coal is overloaded before a pillar line is established, then the abutment zone preceding a line of extraction is no place to split pillars or extract them by any method other than an open-end system. Rice therefore advocated open-end mining, preferably by longwall, but he was willing to compromise with long-face mining if the longwall method was not acceptable. Rice's system was put into operation in a mine in Harlan County, Kentucky,3 but subsequent experience has shown that it did not take into account two important factors—avoidance of pillar-line points and maintenance of adequate development in advance of the pillar-line abutment area. For ten years after Rice's retirement the USBM did little investigation and research on bumps, chiefly because so few were occurring that there was not much cause for alarm. But in 1951 there were three occurrences involving fatal injuries, and the Bureau began a statistical survey in that year. C. T. Holland, head of the department of mines at Virginia Polytechnic Institute, was retained as a consultant. The resulting study' of 117 case histories brought out these important conclusions: 1) Almost invariably the bump occurred in a locality affected by the abutment zones of one or more pillar lines. 2) In most cases the locality of the bump was influenced by the abutment zones of more than one pillar line. The term pillar-line point has been used for many years in the Appalachian region for such a situation. Point is used in the geographical rather than the mathematical sense. 3) In pillar-line extraction the following practices are safest in preventing bumps: a. The mine layout should provide for pillars of uniform size and shape along the extraction line. b. The mine layout should be planned so that no development need be done in the abutment zone of a pillar line. c. The layout should permit open-end extraction of pillar lines from the next goaf, so that it will not be necessary to resort to pocket mining, splitting pillars, or any practice that will involve driving in the direction of the goaf within the abutment zone. d. Pillars should be large enough to support area without undue roof and floor convergence before establishment of a pillar line. These are, of course, generalities, and while they are useful in laying out areas where bumps can be expected, they are of limited help in many mines that were committed to a system of mining before it was realized that they were subject to bumps. Under such conditions it becomes necessary to choose between the following alternatives: 1) Abandon the territory, except for pillars that offer no extraction problems. 2) Through experience select the pillars that are most heavily loaded, and, by augering, induce bumps from a safe vantage point so that impinged loads are relieved. This method was first developed at the Gary, W. Va. mines of U. S. Steel Corp. and later adapted to mining thick coal beds at Kaiser Steel's Sunnyside mine in Utah. No scientific method is available to determine where to drill within a loaded pillar. Although this method of unloading has worked very successfully at Gary—with one exception—

Jan 1, 1959

By A. A. Burr, D. G. Ebeling

The effects of casting texture, grain orientation and grain size upon the performance of Alnico permanent magnets is described. Single-crystal specimens were produced by special sintering and grain coarsening techniques to study the effect of crystal orientation. In addition to texture and orientation effects, an analysis of the results indicates that the permanent magnet performance is impaired by a refinement of the grain size. AN excellent historical review of the development of Alnico permanent magnets has been prepared by Bozorth.1 The desirable permanent magnet characteristics of Fe-Ni-A1 alloys were discovered in 1932 by Mishima.2,3 The work of Ruder' showed that the alloys were age-hardenable, and Betteridge5 defined the best composition and heat treatment for the magnetically isotropic alloy known as "Alnico 3." Horsburgh and Tetley0 increased the energy product by the addition of cobalt and copper, "Alnico 2," and Oliver and Sheddon7 demonstrated that cooling in a magnetic field improved the residual induction of this alloy. Jonas8,9 then disclosed the great practical benefits of heat treating an alloy of higher cobalt content in a magnetic field and the resulting alloy, "Alnico 5," has become the standard of the industry. This paper describes the fundamental aspects of a procedure which can be used to further improve the properties of these anisotropic permanent magnet alloys. A study of the casting techniques used in the production of anisotropic Alnico permanent magnets indicated that the magnetic quality was affected by the as-cast macrostructure. Improved performance was observed in magnets containing a high percentage of columnar grains whose long axes were parallel to the magnetic axis of the casting. McCaig10 studied the effect of such columnar grain structures upon the magnetostriction characteristics of similar alloys, however no data was presented showing the effects on other magnetic properties. The following paragraphs describe two experiments which were conducted to determine the effect of various grain orientations upon the energy product. Special composite molds were prepared of highly conductive and highly refractive components to remove the heat of solidification from the casting in a controlled manner. Representative macrostructures produced by these techniques are shown in Fig. 1, along with the relative volumes of favorably oriented columnar grains. The alloy, Alnico 5, has the highest permanent magnet performance of any commercial magnet material. It has the nominal weight composition of 8 pct Al, 14 pct Ni, 24 pct Co, 3 pct Cu, and 51 pct Fe. A heat of this material was cast into molds producing the type A and B grain structures shown in Fig. 1 and pairs of the resulting magnets were placed in heat-treating boats so as to eliminate any biasing effects of boat position. After a standard heat treatment the type A magnets, with 16 pct of the volume composed of favorably aligned grains, had a maximum energy value of 3,940,000 gauss-oersteds, while the type B magnets with 73 pct aligned grains averaged 5,090,000. This large im-

Jan 1, 1954

At the annual meeting of the American Society of Mechanical Engineers, Dec. 4 to 7, 1917, a great many matters were discussed and acted upon in which nearly all engineers are equally interested. Of the numerous sessions of the meeting, only a few of the most important can be referred too here. The Committee on Gages held an open meeting for the discussion of this important matter. Representatives from a large number of manufacturing plants and from several departments of the Federal Government were present. The question of gages and standardization of mechanical details is of course of paramount interest just now in connection with the manufacture of ordnance and ammunition. After discussion, the following recommendation was adopted by the meeting, for inclusion in all Government contracts for the manufacture of these materials. The maste and reference gages and standards of measurements, with which Ore

Jan 1, 1918

By Secretary

The two papers by Mr. C. M. Rolker, " Notes on Certain IronOre Deposits in Colorado," and "Notes on the Leadville OreDeposits," printed at pages 266 and 273 of this volume, were put to press (owing to the author's absence from the country) without final revision by him. The following corrections are thus made necessary: On page 272, line 13 should read, "respectively 12 and 4 feet" (instead of 12 and 14). On the same page, line 6 from the bottom should read, " the remaining 360 feet" (instead of 320). On page 284, lines 23 and 21 should read, " 111 some places, the dolomite sand roof has remained thicker; and in isolated parts of the bed no replacement has occurred."

Jan 1, 1886

By A. H. Bromly

THE small agricultural village of Santa Barbara, in the State of Guanajuato, has been the center of spasmodic tin-mining operations during recent years. The deposits, so far as I know, are unique, and a few brief notes may be of interest. Santa Barbara, about 12 miles west of San Felipe station on the Mexican National Railway, and at an elevation of 2,400 m. above sea-level, is situated in a flat valley extending east and west, and bounded north and south by broken rugged bills rising about 330 m. above the general level of the valley. Tin-mining operations have been conducted-at the Queensland mine, near this village. A small concentrating-mill was erected and attempts were made to smelt the ore in reverberatory furnaces. The country-rock of the district for many miles is rhyolite of great thickness. There are some local variations due to differences in cooling, or subsequent alteration or impregnation; but throughout the whole district the principal constituents of the rocks remain the same, viz., free silica, orthoclase-feldspar and sanidine. The latter is especially marled. The crevice and joints of the rock are frequently filled with calcedonic and opalescent quartz. The ore-formation at the Queensland mine is of an unusual nature, consisting of cracks in the rhyolite which have been filled with clay. This phenomenon is largely developed over a width of from 80 to 100 m., in which the principal fissuring follows an approximate direction of north and south. The av¬erage clip ranges between 70 to 80 degrees. Some of the fissures bold sufficiently true for a time to afford the impression that they are clue to dynamic causes, or earth-movement. This may be true of some of the north by south fissures; but considering

Jul 1, 1905

By K. D. Jacob, H. L. Marshall, D. S. Reynolds

All types of commercial phosphate rock produced throughout the world contain fluorine in quantities ranging from approximately 0.4 to 1.3 per cent in the Curacao and Christmas Island phosphates to 3.1 to 4.2 per cent in the phosphates of the United States and North Africa1. For a given type of rock, the fluorine content is usually roughly proportional to the phosphorus content. Significance of Fluorine in Phosphate Rock On the basis of chemical and X-ray diffraction studies, Hendricks and co-workers2 concluded that fluorapatite, Cal10F2(PO4)6, is the essential phosphatic constituent of the commercial types of domestic phosphate rock. On the other hand, Bredig and co-workers3 have recently advanced the opinion, also based on X-ray diffraction studies, that the mineral phosphates usually contain carbon dioxide in the apatite lattice, and that the phosphate rocks of the United States are really fluorcarbonate apatites. However, the domestic types of phosphate rock do not seem to differ greatly from coarsely crystalline fluorapatite in their behavior toward chemical reagents in general, and for the purpose of this paper it will suffice to consider fluorapatite as being the essential phosphatic constituent of these types of rock. The available data1 indicate that the different commercial types of domestic phosphate rock usually contain about 12 to 52 per cent more fluorine than theoretically is required to form fluorapatite with all the phosphorus. Calcium fluoride (fluorite) has been definitely identified in only a very few of the samples that have been examined1,2. Bredig and co-workers4 state that fluorapatite can take into its crystal lattice excess calcium fluoride to the extent of approximately 70 per cent of that theoretically required by the formula Ca10F²(PO4)6 without causing more

Jan 1, 1938

By D. S. Reynolds, K. D. Jacob, H. L. Marshall

All types of commercial phosphate rock produced throughout the world contain fluorine in quantities ranging from approximately 0.4 to 1.3 per cent in the Curacao and Christmas Island phosphates to 3.1 to 4.2 per cent in the phosphates of the United States and North Africa1. For a given type of rock, the fluorine content is usually roughly proportional to the phosphorus content. Significance of Fluorine in Phosphate Rock On the basis of chemical and X-ray diffraction studies, Hendricks and co-workers2 concluded that fluorapatite, Cal10F2(PO4)6, is the essential phosphatic constituent of the commercial types of domestic phosphate rock. On the other hand, Bredig and co-workers3 have recently advanced the opinion, also based on X-ray diffraction studies, that the mineral phosphates usually contain carbon dioxide in the apatite lattice, and that the phosphate rocks of the United States are really fluorcarbonate apatites. However, the domestic types of phosphate rock do not seem to differ greatly from coarsely crystalline fluorapatite in their behavior toward chemical reagents in general, and for the purpose of this paper it will suffice to consider fluorapatite as being the essential phosphatic constituent of these types of rock. The available data1 indicate that the different commercial types of domestic phosphate rock usually contain about 12 to 52 per cent more fluorine than theoretically is required to form fluorapatite with all the phosphorus. Calcium fluoride (fluorite) has been definitely identified in only a very few of the samples that have been examined1,2. Bredig and co-workers4 state that fluorapatite can take into its crystal lattice excess calcium fluoride to the extent of approximately 70 per cent of that theoretically required by the formula Ca10F²(PO4)6 without causing more

Jan 1, 1938

By D. E. Norquist, J. E. Moeller

The results of wear on marked balls, 4, 31/2, 3, and 2 in. diam are given. All balls were forged steel of practically the same chemical analysis and hardness. The results indicate that balls in a given mill for a given length of time will have equal diameter losses, regardless of size.

Jan 6, 1950

By Frank Nicholson

Copper ore was first noticed in Ste. Genevieve County in 1563. The diswvery mas made by a German farmer named Simon Grass, who had occasion to make a road from his farm down the hill into the neighboring valley, and while so engaged noticed pieces of a green-colored mineral, some of which he collected. Not knowing the character of the ore he had found, and supposing it to be valua ble for its brilliant green color only, he carried a piece with him into the town of Ste. Genevieve and showed it around the various bar rooms as a curiosity. No special attention was paid to the matter until nine years later, when Mr. 0. D. Harris sent a specimen of the ore to Dr. Theodore Fay, of St. Louis, for analysis. This analysis, which was the first ever made of Ste. Genevieve copper ore, showed the specimen to contain : Copper,. .........17.75 per cent. Zinc,..........3.21 " Iron........... 24.50 " Sulphur ..........1.09 " Organic matter, silica, carbon, and oxygen,. .. 53.45 " 100.00 " From this analysis it is evident that the sample was taken from near the surface, and was probably recognized by its green color. The almost entire absence of sulphur proves it to be an oxidized form. There is on file, at the office of the Ste. Genevieve Copper Works, a paper* giving three arsays of the ore made in 1875 by Henry B.

Jan 1, 1882

By J. S. Kasper, R. M. Waterstrat, B. F. Decker

THE existence of v phase in the Mn-Mo system was discovered in this laboratory several years ago,' but neither the conditions of its formation nor its composition were known, and preliminary attempts to reproduce the phase were unsuccessful. We wish now to specify the information appropriate to phase formation on the basis of experiments performed since that time. The starting materials were in every case electrolytic manganese and high purity molybdenum. Two methods of preparation were employed: l—arc-melting varying combinations of the elements in an inert atmosphere and subsequent heat treating, and 2—sintering compressed mixtures of finely divided powders of the elements. In the latter method, the powders were first passed through 200 mesh screen and then compressed into cylinders of % in. diameter and % in. length, which were sintered at elevated temperatures in an atmosphere of dry hydrogen. For some samples, the sintering temperature was 1200°C (for 1 hr), and these were then heat- treated at lower temperatures for times up to 24 hr. Eventually it was found, for the proper composition, that essentially pure a phase could be produced by sintering at 1125°C for 3 hr. Quenching to room temperature was effected by means of a stream of cold, dry hydrogen in a water-cooled chamber. The arc-melting procedure was found to be unsatisfactory after an investigation of many samples at different compositions and temperatures. Large quantities of manganese were vaporized during melting and none of the products were homogeneous or contained extended regions of pure phase. Nonetheless, these experiments established that no formation occurs in the Mn-Mo system below 1115oC, and indicated, at least roughly, the composition range of interest for further exploration. The more definite results obtained from samples produced by the second method are given in Table I. A portion of sample 2 heated for 16 hr at 1000°C in a Vycor tube transformed to molybdenum plus unidentified phases of complex X-ray pattern. From these few results it appears that the region of phase is quite narrow in composition. It is of interest that the composition is such as to make for difficulties in correlating this structure on an electron atom basis with other a structures of iron, cobalt, and nickel. In that respect Mn-Mo shows the same anomaly as Mn-Cr and Mn-V systems.' A second feature is that in common with the two other known molybdenum (Fe-Mo and Co-Mo), Mn-Mo v exists only at elevated temperatures. The X-ray powder pattern of the pure a phase of Mn-Mo is given in Table 11. It agrees well with the patterns established for other structures, especially with that for Fe-Mo as given by Goldschmidt.An attempt is being made to establish whether an ordering of the respective atoms occurs and such information will be reported in a future publication. Acknowledgment The authors acknowledge gratefully the assistance of Mrs. J. R. Belanger in some portions of this work. References 'J. S. Kasper, B. F. Decker, and J. R. Belanger: Journal of Applied Physics (1951) 22, p. 361. 2 A. H. Sully: Journal Inst. Metals (1951) 80, p. 173. H. J. Goldschmidt: Research (1949) 2, p. 343.

Jan 1, 1954

By J. H. Jensen

Bromine is the intermediate member of the halogen family of elements between iodine, a solid: and chlorine, a gas. The name is derived from the Greek "bromos," meaning stench. Bromine is the only nonmetallic element that is liquid at room temperatures with a melting point of -7.2" C and a boiling point of 58.78" C. Reddish brown in color, it dissolves easily in water to yield a red solution. Bromine volatilizes at ordinary temperatures to a red vapor that is very irritating to the eyes, nose, and throat. Density of the liquid is 3.12 and gas weighs 7.59 gpl at standard conditions. As the element is highly active, it exists in nature only as bromide compounds. Bromine was discovered by Antoine Jerome Balard in seawater bitterns in 1826 and first prepared in quantity in 1860. Distribution Bromine is widely distributed in nature and compounds occur in solution in natural brines, in seawater, saline lakes, oil and gas well brines, and in evaporite chloride minerals. The concentration of bromine salts ranges from 60- 65 ppm in seawater to several thousand ppm in oil well brines and saline lakes. The distribution of bromine in marine evaporite minerals and in the solutions from which they crystallized was determined many years ago by H. E. Boeke (1 908). Theoretical aspects regarding the geochemistry of bromine have been published in numerous papers (Raup and Mite, 1969). Bromine occurs in solid solution in carnallite and sylvite associated in potash de- posits; in halite in salt beds; salt in oil shales; and in trona deposits. Its presence is useful as a guide in geochemical exploration. The analysis of small amounts of bromides in the presence of large amounts of chlorides is discussed by W. Schwerdtner (1963). Manganese, iron, and iodine may interfere with the determination. Other analytical methods are discussed at length in the literature (Stenger and Atchison, 1964). Sources and Reserves The sources and reserves of bromine, given in [Table 1], appear ample to meet present and foreseeable requirements in all producing countries. With the occurrence of bromine salts in sea-water and other brines, the potential for bromine production is worldwide. It has been estimated that 99% of all commercially recoverable bromine is in the ocean. However, actual subterranean brines having a higher bromine content than seawater will continue to be the preferred sources of bromine for the foreseeable future. Markets and Prices About 17% (1968) of bromine produced is used in its elemental form, with the balance consumed as bromides and bromates. The largest use for bromine is ethylene dibromide which, together with tetraethyl lead, are used as an antiknock additive in gasoline. Tetra-ethyl lead is the antiknock agent. Ethylene dibromide combines with the lead after combustion in the engine to form a volatile com- pound that escapes from the engine with the exhaust gases.

Jan 1, 1975

By D. Mills, G. B. Craig

ZIRCONIUM has been float-zone-refined in an electron-beam furnace and the redistribution of oxygen, iron, and tungsten has been measured. The iodide zirconium used in the present experiments initially contained both oxygen and iron in the range 100 to 200 ppm by weight, and tungsten in amounts less than 10 ppm. Float-zone refining of zirconium, using induction heating, has previously been attempted by Kneip and Betterton1 and Langeron.2 Kneip and Betterton were primarily interested in the removal of iron and nickel. They achieved some purification, with respect to both these elements, in material given up to six passes at 150 mm per hr under an argon atmosphere. Langeron reported purification for a large number of elements after four completed passes in a static vacuum system operating at pressures less than 10-6 mm of Hg and with rates of zone travel between 30 and 40 mm per hr. He did not report oxygen concentrations, but stated that there was inverse segregation of this element. westlake5 has also used a minimum of four zone passes to remove iron from zirconium. No rates or conditions were given. Belk6 has shown that tungsten contamination can occur during electron-beam melting. He reported an increase from 0.01 to 0.05 pct by weight tungsten in molybdenum after four complete zone passes. The vacuum system for the electron-beam unit used in the present investigation consisted of a single-stage rotary pump backing a liquid-air-trapped oil-diffusion pump. A pressure of less than 10-8 mm of Hg was obtained with Dow-Corning 705 fluid in the diffusion pump. In order to avoid contamination of the zirconium by evaporation from the tungsten filament, a special focusing cage4 was employed. Three rates of zone travel, 114, 38, and 4 mm per hr, were investigated, with the liquid zone moving from the bottom to the top of the bar. The bars used were 3 mm diam and the total melted length was 130 mm. Oxygen was analyzed by neutron-activation analysis using a neutron flux of 10' neutrons per sq cm per sec to form the isotope N16 by the 016 (n,p) N16 reaction. The standard deviation is quoted for each oxygen determination. The iron and tungsten analyses were performed spectrographically, and the precision is estimated to be ±6 pct. Analyses for tungsten were all below the detectable limit of 10 ppm, confirming the protection given by the focusing cage. No significant redistribution of oxygen was found at the two higher rates of zone travel. The redistribution of oxygen and iron obtained after five passes at a rate of zone travel of 4 mm per hr (1.1 x 10-4 cm per sec) is recorded in Tables I and 11. Burris, Stockman, and Dillon3 have estimated the distribution of solutes during multipass zone refining. Using their curves for an effective distribution coefficient of Keff = 1.5 and 2 for oxygen and Keff = 0.3 for iron, the expected concentrations were estimated for the present material. These are shown in Tables I and 11, along with the experimentally measured values. The calculated concentrations are based on a molten-zone length of 10 pct of the total melted length, whereas in the present experiments the molten zone was approximately 5 pct of the total melted length. The effect of zone length on solute redistribution is most pronounced after a large number of zone passes. Comparison with Pfann's published data8 for solute redistribution for various Keff's and zone lengths indicates only small differences at low numbers of completed zone passes. It is evident that the expected distribution has not been realized in the case of iron. Scrapings of material deposited on the inner surfaces of the electron-focusing cage were found to be magnetic. It is, therefore, concluded that redistribution of iron is masked by evaporation. Deposition of iron inside the focusing cage was observed at all rates of zone travel. The results of the investigation may be summarized as follows: 1) Segregation of oxygen is typical for a solute with a distribution coefficient, Keff > 1. 2) No redistribution of oxygen takes place at high rates of zone travel. 3) The distribution coefficient for oxygen lies between 1.5 and 2.0. 4) Purification with respect to iron occurs mainly by evaporation. 5) The focusing cage is effective in preventing tungsten contamination.

Jan 1, 1967

By F. J. Martin, W. G. Hubler

The Beattie mine is at about the center of Duparquet township in the Province of Quebec, Canada. It is 22 miles northwest of the town of Noranda. The elevation is approximately 1200 ft. above sea level. This locality, long considered a favorable one from the geological point of view, has been prospected for over 20 years, but no discoveries of economic importance were made until the present orebody was found by John Beattie in 1930. The specific gravity of the ore is 2.77. The gold occurs in intimate association with the sulfides, pyrite and arsenopyrite, which in turn are very finely disseminated in a silicified porphyry. The bulk of the gold is associated with the pyrite, only a small proportion being with the arsenopyrite. There are small amounts of magnetite, ilmenite and chalcopyrite present in the ore. There is also some hematite in the ore that is mined from near the surface in the open pit. Metallurgical Problems and Methods or Attack 1. The ore is extremely hard and resistant to grinding. 2. The sulfide minerals are finely disseminated in the gangue. 3. The gold, in turn, is so intimately associated with the sulfides that grinding to even 5 microns will not release all of the values for cyanidation. 4. It is necessary to make a high ratio of concentration in order to obtain a product sufficiently high in gold to meet high shipping and treatment charges. Hardness of the Ore.—Owing to the extreme resistance of the ore to grinding, it was recognized that grinding costs would be high. Microscopic tests showed that grinding to 95 per cent minus 325 mesh would be necessary to liberate a sufficient amount of the values in order to obtain a tailing assaying 0.02 oz. gold per ton, which is considered to have the economical minimum gold content that can be obtained. It is not feasible to grind this hard low-grade ore (0.18 to 0.20 oz.) to 95 per cent minus 325 mesh, so it was necessary to overcome the problem in another way. The following method was decided upon: (1) Fine crushing to minus 1/4 in.; (2) relatively coarse primary grinding; flotation of low-grade concentrates in the primary and rougher circuits and discarding the

Jan 1, 1935

By L. D. Jaffe, H. C. Mann, E. L. Reed

The authors have recently published1 evidence that brittle transgranular fracture of polycrystalline metals does not originate at a point and propagate continuously across the material, but rather develops at numerous related points, leading to a series of micro-cracks which subsequently link up. Series of related microcracks were observed in steel specimens broken in fatigue—specifically, at the central portions which broke during the final sudden fracture. Microcracks of the type mentioned have also been reported by Baeyertz, Craig and Bumps'2 in steel broken under impact. % Some micrographs published by Irwin3 may possibly be interpreted as showing discontinuous brittle cracks. This paper presents additional observations of the authors on discontinuous crack propagation under various conditions. Impact Test Specimens The impact test specimens were cut longitudinally from a steel forging containing: The heat treatment consisted of oil quenching in a heavy section from 1600°F and tempering at 1260°F. The resulting yield strength was 78,000 psi, tensile strength 100,000 psi, elongation 20.0 pet in 2 in., and reduction of area 55.0 pet. Standard V-notch Charpy specimens were broken in a 217 ft-lb machine at a striking velocity of 16.8 fps. Energy absorption and fracture appearance of this material in the V-notch Charpy test are plotted as functions of temperature in Fig 1. After test, fractured halves of specimens appearing 0, 40, 80, and 100 pet fibrous (to the unaided eye) were electroplated with nickel, sectioned longitudinally (perpendicular to the notch at its midpoint), polished and etched with Cohen-Hurlich-Jacobson (C-H-J) reagent (picric acid plus Zephiran chloride in ethyl ether)4 or with Vilella reagent (1 pet picric plus 5 pct hydrochloric acid in ethyl alcohol).5 Fig 2 and 3 show cracks near the path of final fracture in the specimen rated 0 pct fibrous. Many of the cracks terminate at the boundaries of ferrite grains, some at boundaries of pre- existing austenite gzains. * A crack often starts near the end of another. Cracks within the same ferrite grains are parallel or approximately parallel in several cases. A large percentage of the cracks are branched. Fig 4 illustrated a group of cracks in the 40 pct fibrous specimen. Branching and parallelism are well marked. No more than three directions of crack have been observed on the polished surface in one ferrite grain. This is consistent with the evidence6 that brittle fracture of ferrite takes place on the cube face crystallographic planes: the {100} planes. The appearance of some cracks suggests that they have passed around a projecting corner of a second ferrite grain by going outside the plane of polish. In Fig 5 cracks in the 80 pet fibrous specimen may be observed. Some of

Jan 1, 1950

By Oren C. Baptist, Eliot J. White

Samples of four reservoir sands having different degrees of water sensitivity were subjected to several laboratory tests to determine differences in capillary behavior attributable to clay-mineral effects. The degree of water sensitivity was estimated by the difference between gas and water permeability. Unsaturated pore volumes determined with mercury injection were comparable to irreducible water saturations determined with the semipermeable bar-rier method only for the non-sensitive sands that contained small amounts of non-swelling clay minerals. Irreducible saturations were independent of salinity of the water, which suggests that most residual water is adsorbed 0.7 a film over solid surfaces and that internal retention by clay minerals is relatively insignificant. The water-sensitive sands imbibed water to higher saturations than did non-sensitive sands, and this result is believed to be a combination of the effects of clay minerals and preferential wettability; however, the relative importance of each of these effects is riot determinable. Thus it is concluded that the semipermeable barrier method is the best of the laborafory methods used for estimating formntion water .saturations in the sands studied. INTRODUCTION This investigation is a continuation of studies of the role of clay minerals in petroleum production in the Rocky Mountain area. Previous work has shown large differences in gas and water permeability in numerous reservoir sands; these water-sensitivity effects observed in the laboratory have been correlated with well behavior in the field, and the degree of water sensitivity imparted to reservoirs by the various clay minerals has been determined.'.' The effect of interstitial clay minerals on formation water3 saturations is not so well known. It has been reported that formation water saturations probably are higher in clayey than clean sands,' but this effect has not been evaluated in the laboratory, and the relative effect of the various types of clay minerals on formation water saturation has not been determined. The clay-mineral groups of most importance to this study and to petroleum production in general are kaolinite, illite, and montmorillonite. The minute layers of montmorillonite are loosely bound to one another so that water enters between them, causing great expansion of the particles. Kaolinite and illite do not exhibit interlayer hydration, but they do immobilize considerable amounts of water owing to their large surface areas, which are of the order of 15 to 97 m2/gm of clay.5 The four Wyoming sands used in this study were selected to represent a wide range of water sensitivities. These sands, with the number of wells and fields from which the samples were obtained, are: Second Frontier, five wells in two fields; Newcastle, six wells in one field; Tensleep, two wells in two fields; and Lower Muddy, five wells in one field. EXPERIMENTAL METHODS AND PROCEDURES Water-displacement data were obtained by the semipermeable barrier method," using both fresh water and brines having either 16,500 ppm sodium chloride or calcium chloride. A displacement pressure of 35 psi was found to be sufficient to obtain the practical irreducible water or brine saturation (IWS, IBS) in most samples. Mercury-injection data were ob-tained with equipment and pro-cedures similar to those described by Purcell.7 Exceedingly high pressures are required to attain complete mercury saturation by this method; however, since saturations in most samples change very little with large pressure increases above 1,000 psia, the maximum pressure used was 1,400 psia. To facilitate comparison of mercury-injection and water-displacement results, it is convenient to express mercury-injection data in terms of unsaturated pore volume. The abbreviation, (100 - SHg)min, is used to denote the pore volume unsaturated by mercury at 1,400 psia injection pressure. Gas permeabilities, ki, were deter-mined by the method proposed by Klinkenberg.8 Methods of determining types and amounts of clay minerals by X-ray diffraction analyses, as well as methods of determining water permeability, have been described previously.' The imbibition characteristics of

Jan 1, 1958

By AIME AIME

AT A meeting of the Boston Local Section of the Institute, on Oct. 3, approval was voted to the work done by its representatives on the Committee opposing the passage of a bill by the, Massachusetts Legislature to license engineers. The report is as follows: The Joint Committee on Licensing of Engineers, which included a Committee of the Boston Society of Civil Engineers and representatives of seven other societies,* submitted to the members of the respective societies, on Jan. 8, 1921, a report in which it was stated that on Jan. 4, 1921, a petition was filed in the Legislature of Massachusetts by the Boston Chapter of the American Association of Engineers accompanied by a bill to provide for the registration of professional engineers and land surveyors. This report also stated that at a meeting of this committee, held on Jan. 7, 1921, it was voted:

Jan 1, 1921

By Heinrich Ries

The manufacture of fire-brick represents one of the oldest branches of the clay-working industry in New Jersey, and is of more importance than is commonly imagined. The New Jersey clays were first used for fire-brick after the war of 1812, and one of the earliest records, according to Professor Cook, shows that clay was taken from Woodbridge to Boston in 1816, arid used for that purpose. The value of the clays of the Woodbridge district does not seem to have been well and widely recognized for some years, however, although in 1855 the statistics, given in the Geological Report, show that clay for making 50,000,000 fire-bricks was then taken annually from the pits at Woodbridge, Perth Amboy and South Amboy. Perhaps the oldest works in the State was that known as the Salamander works (no longer in existence), where brick were made as early as 1825. A little later, in 1836, John R. Watson established a factory at Perth Amboy, and in 1858 Sayre & Fisher began the manufacture of fire-brick at Washington. The works of W. H. Berry at Woodbridge began operations in 1845, and have continued up to the present clay, although in 1896 the name was changed to J. E. Berry. The works of Henry Maurer & Son were established in 1856, and those of M. D. Valentine & Brother in 1865. These latter were started for making bath brick; later, sewer-pipe, and, finally, fire-brick and other refractory shapes were produced. A branch-works, located at Valentine on the Central railroad of New Jersey, was started in 1887. Even in the last two years several works have begun the manufacture of fire-brick. These include factories erected by

Jan 1, 1904

By Kent R. Van Horn, W. P. Sykes

Since Honda and Murakamil in 1918 proposed their constitutional diagram of the carbon-free iron-tungsten system, considerable effort has been expended by several investigators in attempts to define more positively the structural features of the alloys. The existence of an intermediate phase corresponding to the formula Fe3W2 (68.7 per cent W) was proposed from evidence of a purely metallographic nature by one of the present authors2 in 1926. Since that time the identity of this phase has been confirmed by Arnfelt3 and by Takeda,4 both of whom employed X-ray methods as well as the microscope and the chemical analysis of isolated microconstituents. According to Arnfelt, Fe3W2, as crystallized from the iron-rich melts at a temperature above 1450° C., contains by analysis 68.7 per cent W. The lattice of this phase is characterized by trigonal symmetry. Arnfelt, moreover, proposed a second intermediate phase formed at some temperature between 1450" and 1000" C. by a peritectoid reaction involving Fe3W2 and the iron-rich solid solution. A melt containing 25 per cent W was cooled to 1000" C. and heated for 100 hr. The precipitated tungsten-rich constituent was separated and found by analysis to contain 62.6 per cent W. This composition agrees closely with that represented by the formula Fe2W (62.2 per cent W). Diffraction patterns from the concentrated precipitate showed a hexagonal unit cell. Takeda confirmed the data of Arnfelt regarding Fe3W2 but was unable to detect Arnfelt's second intermediate phase. While Takeda failed to describe in detail the treatments employed, he stated that in alloys containing 40 per cent W which were quenched after heating at various temperatures between 1200" and 1450" C. no evidence of the second phase (Fe2W) was observed 'either in the microstructure or in the diffraction patterns of isolated residues. He therefore considered the existence of this low-temperature hexagonal compound as disproved.

Jan 1, 1933

By C. A. Stickels

A heat of electrolytic iron, to whzch alunzinutn and nitrogen had been added, was hot-rolled, cold-rolled 90 pct, and recrystallized at temperatures from 500" to 700°C. Primary recrystallization textures appear to arise from competitive growth of two types of nuclei: 1) those having orientations belonging to the "usual" primary recrystallization texture found in riming steel, and 2) those with the {111} (110) ovientation. Development of a (111}(1 10) component in the primary recrystallization texture occurs only over a certain interval of isothermal recrystallizatzon temperatures when the material is supersaturated with respect to the precipitation of AlN. Lowering the degree of supersaturation depresses the temperature interval in which a (111)(110) component occurs. An elongated, 'pancake-shaped" recrystallized pain structure and a marked delay in the start of recrystallization were found in all specimens which were supersaturated with respect to A1N precipitation after cold work, regardless of their recrystallization texture. ONE of the consequences of killing low-carbon steel with aluminum is a significant change in recrystallization behavior. About 15 years ago, Solter and eatttiel showed that this behavior was largely controlled by aluminum and nitrogen in the steel. If complete precipitation of A1N was prevented before cold rolling, an increased "recrystallization temperature" was observed in subsequent. annealing, and the recrystal-lized grains were not equiaxed. Leslie et a1.2 studied this phenomenon in some detail and clearly demonstrated the relationship between A1N precipitation, recrystallization kinetics, and the development of "pancake-shaped" grains. It has also been known for some time that aluminum-killed steels, processed to produce elongated "pancake" grains, develop a (11 I}( 110) primary recrystallization texture. This texture has not been found in iron or low-carbon rimming steel as a primary texture4j5 but has been observed following grain growth in electrolytic iron.5 The present work was undertaken to study in more detail the effect of A1N supersaturation on recrystallization textures in iron. LITERATURE REVIEW The deformation texture in heavily rolled iron has been studied in detail by Bennewitz.~ The texture consists primarily of a partial fiber texture about a (110) axis in the rolling direction, designated here as fiber texture A. It includes the range of orienta- tions (111)[110] - (001)[ 110] - (11l)[110]. A weak secondary texture also is present.6 This is a duplex partial fiber texture about two (110) fiber axes located 60 deg from the rolling direction and 30 deg from the sheet normal. The range of this texture, designated here as fiber texture B, about the [101} fiber axis is (112)[110] - near (545)[252] - (211:1[011] *The range given here follows Bennewit~.~ A few pole figures from re-crystallized material indicate a broader range than this.' However, the components which are strongest in the recrystallization texture are in this range.'________________________________________________________ Primary recrystallization textures in unkilled steels can be accounted for by growth of members of fiber texture B present in the deformed metal.5 However, while members of fiber texture B dominate the primary texture, other orientations survive primary recrystallization as well. In particular, some {111}(110) members of fiber texture A must also grow during primary recrystallization, because a well-defined {1ll)( 110) texture develops during subsequent grain growth at 700°C.5 The unusual recrystallization behavior of deformed supersaturated solid solutions has been attributed to: 1) retention of the solute in solution,' 2) formation of coherent, preprecipitation solute clusters prior to and during re~r~stallization,~ and 3) formation of a precipitate prior to and concurrent with recrystallization.'~-'~ When aluminum is supersaturated with iron, the difference in grain boundary mobility between general high-angle boundaries and certain special coincidence site boundaries is apparently eliminated.' In aluminum-killed steels, precipitation of A1N can take place at ordinary subcritical recrystallization temperatures. The rate of precipitation increases with increasing aluminum or nitrogen contents.2'13 There is some doubt, however, as to whether true precipitates form during the time at temperature needed to complete recrystallization. Leslie ef a1.2 found that precipitation in one steel was complete after about 100 min at 700GC, or after about 1000 min at 650GC, as measured by chemical analysis for AlN. Aoki et a1.,13 using internal friction for dissolved nitrogen, showed that a large fraction of the dissolved nitrogen was removed from solution within a few minutes annealing time at temperatures from 400" to 800°C. However , the rate of formation of AlN, as detected bv chemical analvsis. was much slower than the apparent rate of nitrogen removal. Hasebe,'~~ using carbon extraction replicas, has identified A1N precipitates by electron diffraction in a 0.2 C steel, solution-treated at 1300°C and annealed 2 hr at 700°C. Borchers and kim,I6 also using a replication technique, observed precipitates after annealing treatments as short as 2 min at 640°C. However, Leslie et a1.' state that no A1N precipitate can be seen while recrystallization is being inhibited in aluminum-killed steel.

Jan 1, 1967