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By J. F. Butler

Boron nitride, BN, has been identified in boron low-carbon steels by means of light microscopy, electron microscopy and diffraction, and chemical analysis. This boron nitride is responsible for strain aging suppression in these steels through the removal of nitrogen from solution; however, small oxidizing potentials which result in deboronization In the austenitic temperature range also result in boron nitride decomposition and the subsequent occurrence of nitrogen strain aging. THE addition of boron to low-carbon steels is an effective means of eliminating the detrimental effects of strain aging;',' however, the mechanism by which boron suppresses strain aging has not been established. In studying the effect of heat treatment on the strain aging of boron low-carbon steels, Butler3 found that no detectable nitrogen was present in the ferrite solid solution after various heat treatments even though the total nitrogen analyses of the steels were 0.003 pct N. Apparently the function of boron in suppressing strain aging is the removal of nitrogen from solution to form a relatively stable second phase. A clue to the identity of this phase was found by Speight4 who extracted from an aluminum-killed boron steel an acid insoluble residue which contained boron and nitrogen in proportions corresponding to the compound, BN. Shyne and Morgan5 found that the addition of nitrogen to a hardenable boron steel lowered its hardenability in a manner which suggest-d the presence of nucleating particles (presumably BN) even at high austenitizing temperatures. Although this indirect evidence for the presence of boron nitride in boron steels has been found, the compound was not identified metallographically as a separate phase in these steels. Because boron has an affinity for oxygen comparable to that of silicon,5 boron steels must be thoroughly killed with aluminum in order to prevent the reaction of boron with oxygen.7 The affinity of boron for oxygen also is demonstrated through the ease of deboronization of a boron steel in an oxidizing atmosphere. Digges, Irish, and Carwile8 found that a mixture of wet natural gas and air caused both deboronixation and decarburization of a boron steel at 1900°F. The boron content rose at the surface of the steel due to the formation of boron oxide. Shyne and Morgan9 encountered deboronization at much lower oxygen potentials; loss of boron occurred in steels treated at 1750o F under argon purified to 0.0014 pct 0, even though decarburization did not occur. Boron oxide, B2O3, is much more stable than the nitride, BN, as is indicated by the standard free energies of formation at 980oC: -235 kcal per mol of B2O3 (liquid) and -28 kcal per mol of BN (crystal). It is evident that the oxygen potential must be kept low in the presence of BN in order to prevent its decomposition and the subsequent formation of B2O3' The purpose of the work described in this paper was to identify the nitride phase responsible for the removal of nitrogen from solution and to study its stability under oxidizing conditions. IDENTIFICATION OF BN In order to identify the phase containing boron and nitrogen, several alloys high in boron and nitrogen were made up in a small vacuum furnace. In alloys 3 and 4, Table I, electrolytic iron was used as a charge material. Boron additions were made in the form of 18 pct B ferro-boron after the iron was molten. In the case of alloy 3, the charge was solidified at this point; for alloy 4, nitrogen at 1 atm pressure was admitted over the melt before it was

Jan 1, 1962

By W. B. Tijmann

Maintaining safe, yet economical, slope geometries in a mining operation is paramount. When design analysis and engineering judgement have dictated conservative and usually more expensive problem solutions, monitoring has often proven to be a valuable method in dealing with potential slope instability. A well planned and executed monitoring program can allow operation at a lower theoretical margin of safety. Monitoring provides a valuable check on design parameters and can measure effects of remedial improvements. Warning of impending failure can often be established well in advance. The monitoring problem situations in civil engineering works and open pit mining are much alike. Instruments used for monitoring in both industries are often the same. In this paper, geotechnical instruments for measuring deformation and groundwater pressure in rock and overburden are discussed with a broad-brush approach. Results obtained over extended time periods are presented in a graphical presentation for a case history. Descriptions of various types of instruments, mostly used to monitor stability of rock slopes, are discussed, and data analysis and approximate costs are presented.

Jan 1, 1983

By W. M. Bertholf

IN 1945 tests were made in the coal washery of the Colorado Fuel and Iron Corporation, at Pueblo, Colo., to determine the value of the Humphreys spiral. So far we have demonstrated that it is of definite value to us in rewashing a portion of our table middlings; and we are fairly certain that this is not necessarily the only place in which it can be used to advantage. Because of manpower and material shortages, experimental work has been discontinued for the present. Three of the spirals are being installed for use in rewashing the middlings, and testing and experimental work will proceed when this installation is completed. All evidence secured so far points to the fact that the spiral can make an effective separation of heavy material below 8-mesh; but that it is ineffective in removing larger, heavy material. This, of course, will limit its use to fine coal or a classified feed containing no heavy material larger than 8-mesh. In considering the results of our tests, it should be noted that the feed was our table middling, and that any real separation of this material is a "moral victory," as there is little material that could be properly called coal and practically no heavy rock, the consequence being that previous attempts to clean the middlings have not been at all successful. Several articles dealing with the spiral and its use in treating heavy minerals have already been published,1 but for the benefit of those who have not seen these we include a brief description of the spiral and of the way it operates, taken from Bulletin 4 of The Humphreys Investment Co.: The Humphreys Spiral Concentrator consists of a spiral conduit of modified semicircular cross section. Ore pulp is fed to the top and, as it flows downward, the heavier particles concentrate in a band along the inner side of the pulp stream (Fig. I). Outlets for removal of products are located at the lowest points in the cross section of the conduit. Wash water, added at the inner edge of the stream, flows outwardly across the concentrate band. The width of concentrate band removed at the outlets is controlled by adjustable splitters. Concentrate is usually removed from the upper portion of the spiral and middling from the lower portion. Tailing is discharged from the lower end. Tests are usually made in closed circuit, since this provides a maximum of information with a minimum amount of sample. Fig. 2 shows the spiral set up for closed-circuit testing, and gives a good idea of the general arrangement of such an installation. The small cyclone separator is used to provide clean wash water without introducing additional water into the circuit.

Jan 1, 1946

By George M. Fowler, Joseph P. Lyden

PaGE Scope of this Report.................................................... 206 Production of Tri-State District.......................................... 207 Historical Sketch....................................................... 207 Location and Topography............................................... 211 Geology............................................................... 212 The Tri-State District.............................................. 214 Stratigraphy........................................................... 217 General Geological Section in Tri-State Region....................... 217 Stratigraphic Section of Mineralized part of Boone Formation........... 218 Stratigraphic Section Bird Dog Well.................................. 219 Metamorphism........................................................ 220 Structure............................................................. 225 Regional.......................................................... 225 Due to Metamorphism.............................................. 229 Ore Deposits.......................................................... 231 Types............................................................ 232 Hard-ground Deposits.......................................... 232 Brecciated................................................. 232 Stratified............................................ 232 Sheet Ground............................................. 232 In Dolomite............................................... 233 In Shale.................................................. 233 Soft-ground Deposits.......................................... 233 In the District as a Whole....................................... 233 Ore Minerah and Analysis......................................... 233 Paragenesis....................................................... 234 Conclusions........................................................... 236 Structure.......................................................... 236 Genesis of the Ore.................................................. 237 Future of the District............................................... 239 Acknowledgments..................................................... 239 Discussion............................................................ 239 Scope of This Report The Tri-State district. as outlined in this paper. refers to the entire mineralized area in sout'hwestern Missouri. southeastern Kansas and

Jan 1, 1932

By J. F. Enrietto

It is shown that one cannot approximate the broad internal friction Peaks observed in the Fe-Mn-N system as the sum of a number of subsidiary Peaks and still vetain the concept of a single relaxation time. Furthermore, the approximation of manganese affectirg only nearest neighbor interstitial sites is shown to be incompatible with the experimental results. The results of this experiment show that the influence of manganese in the ferrite lattice extends over 3 to 4 atomic distances. NUMEROUS experiments have shown that the presence of relatively small amounts of substitutional alloying elements can profoundly affect the profile of the damping spectrum in the vicinity of the Snoek peak in bee metals.1-7 Dijkstra and Sladekl observed this phenomenon in Fe-Mn-N alloys where it appeared as a broadening and shifting of the Snoek peak to higher temperatures. The authors interpreted this as being the result of a superposition of two damping maxima—the normal Snoek peak, located at its usual position and having a normal half-width, and an interaction peak having a normal half-width, but occurring at a somewhat higher temperature. They prclposed that the interaction peak was caused by nitrogen atoms jumping from Fe-Mn sites to Fe-Fe sites, the Fe-Mn interstitial sites having one manganese and one iron atom as nearest neighbors, and the Fe-Fe sites having two iron atoms as nearest neighbors. They further suggested that the Fe-Mn sites had a lower energy than the normal Fe-Fe sites because of the presence of the adjacent manganese atoms. From the relative heights of the two postulated damping peaks, the dif-

Jan 1, 1962

By D. V. Carter, F. M. Hackbusch

Beginning the year 1938, the East and East Central Texas district comprised 48 counties, which is equivalent to the Texas Railroad Commission districts 5 and 6. At the close of the year there were 46 oil and gas fields in this district. Eight other fields, seven oil and one gas, have been abandoned. Exploratory Drilling During the year, 113 exploratory wells were drilled. Nine discoveries were made, five of which proved to be oil fields, three distillate, and one gas. Completions for the district were 2043 oil wells (distillate wells included), 36 gas wells and 163 dry holes. Exclusive of the East Texas field, the Marion County extension of the Rodessa field led the district in the number of completions during the year. Production and Proration All fields in the district produced a total of 182,369,484 bbl. of oil, a decrease of 12.57 per cent compared with the 208,594,453 bbl. produced during 1937. The East Texas field produced 148,189,913 bbl., which was 81.6 per cent of the district's production for 1938. November daily average oil production for the East and East Central district was 469,102 bbl. The estimated cumulative production to Jan. 1, 1939, for this district was 1,753,894,802 bbl. It is estimated that the East and East Central district produced 38.9 per cent of the state's total production for the year, which was 468,781,632 barrels. The decrease in 1938 production, as compared to that of 1937, in this district was partly due to the Saturday and Sunday shutdowns, 71 days for the year, which is equivalent to 19.45 per cent of the year. All fields in this district were affected by shutdowns except the Texas portion of the Rodessa field, which was shut in only during January and February. Certain wells were exempt from these shutdowns because of special pro-

Jan 1, 1939

By D. V. Carter, F. M. Hackbusch

Beginning the year 1938, the East and East Central Texas district comprised 48 counties, which is equivalent to the Texas Railroad Commission districts 5 and 6. At the close of the year there were 46 oil and gas fields in this district. Eight other fields, seven oil and one gas, have been abandoned. Exploratory Drilling During the year, 113 exploratory wells were drilled. Nine discoveries were made, five of which proved to be oil fields, three distillate, and one gas. Completions for the district were 2043 oil wells (distillate wells included), 36 gas wells and 163 dry holes. Exclusive of the East Texas field, the Marion County extension of the Rodessa field led the district in the number of completions during the year. Production and Proration All fields in the district produced a total of 182,369,484 bbl. of oil, a decrease of 12.57 per cent compared with the 208,594,453 bbl. produced during 1937. The East Texas field produced 148,189,913 bbl., which was 81.6 per cent of the district's production for 1938. November daily average oil production for the East and East Central district was 469,102 bbl. The estimated cumulative production to Jan. 1, 1939, for this district was 1,753,894,802 bbl. It is estimated that the East and East Central district produced 38.9 per cent of the state's total production for the year, which was 468,781,632 barrels. The decrease in 1938 production, as compared to that of 1937, in this district was partly due to the Saturday and Sunday shutdowns, 71 days for the year, which is equivalent to 19.45 per cent of the year. All fields in this district were affected by shutdowns except the Texas portion of the Rodessa field, which was shut in only during January and February. Certain wells were exempt from these shutdowns because of special pro-

Jan 1, 1939

By H. A. Bauman, T. S. Spicer, C. C. Wright

Experimental data are presented showing the influence of size consist and firing rate upon the performance of bituminous coal-fired, single-retort, industrial underfeed stokers. Size segregation, degradation, and distributor data are also included. The conclusion is reached that size consist of the fuel as fired, is a critical factor in its performance on this class of equipment.

Jan 2, 1950

By W. N. Roberts

Hadfielcl steel has been studied by transmission electron microscopy to determine the microsl.rtic-ture of the cold-worked material, which has been a subject of controversy for many years. The presence of fcc deformation twins in specimens deformed in tension, by hamnzering, and by explosive -shock loading at room temperature lzas been established by electron diffraction. No evidence of a mar tensite was detected in any of the speciwens. Small amounts of E martensite were idenLified in the hamnleved specimens. DESPITE numerous researches on Hadfield steel since its discovery in 1882, there is still disagreement on the nature of transformations in the cold-worked material. Collette el al.,' using X-ray and electron diffraction, have found evidence for stacking faults, E martensite, and a martensite in Hadfield steel deformed in tension at room temperature. Nishiyama and Simizu,' using electron microscopy, have found stacking faults and E martensite in hammered Hadfield steel. White and Honeycombe have concluded from X-ray diffraction that Hadfield steel remains fully austenitic even after severe cold work at -196 Previous work by the author, indicating the presence of a, martensite in deformed Hadfield steel, was in error due to a faulty interpretation of the electron-diffraction patterns. Various workers,5'7 over the years, have speculated on the presence of deformation twins in Hadfield steel, largely from such circumstantial evidence as the persistence of slip bands with repeated polishing and etching, the presence of serrations in the stress-strain curve, and the absence of evidence of a martensite by X-ray measurements. The advent of electron-transmission microscopy and se- lected-area diffraction has made possible the positive identification of fine deformation twinning. PROCEDURE For tensile tests, standard ASTM specimens of 2-in. gage length, ground from 0.12-in. Hadfield steel sheet, were solution-treated at 1050°C for 30 min in a salt bath, to avoid decarburization, and water-quenched. The grain size was about 0.01 sq mm. Chemical analysis of the steel after heat

Jan 1, 1964

By Charles M. Rolker

THIS remarkable and well-known district lies about 320 miles south of Salt Lake City, in Washington County, near the Arizona border of the territory. It is now reached by the Utah Southern Railroad and its extension, and the last 100 miles are run by stages. These vehicles are called "jerkies" in the West, which name conveys a good idea of the comfort they afford, and the relief experienced when you alight. Arriving at Silver Reef, the main amp of the district, one sees at once that he stands where once a surging sen had its domain, marked now by heavy sandstone deposits of a red and white color. The town itself, a neat, clean, and orderly mining town, is encircled on the north by trachyte and granite mountains, skirting to the west. They are cut through in places by deep gorges, left US as the only brace of the force of former currents, which drained the adjoining territory to the north; and which when swelled and infuriated by tempests and cloud-bursts, took in their grasp the huge blocks of

Jan 1, 1881

By Walter Kauenhowen

Germany's crude oil production during 1935 totaled 3,007,711 bbl., an increase of 36.6 per cent over the 2,202,214 bbl. produced in 1934. The Nienhagen-Haenigsen field furnished 77 per cent of the total 1935 production. Cumulative production figures for Germany's two most important oil fields, Wietze and Nienhagen, show that during the period from 1872 to the close of 1935 the Wietze field produced 13,325,536 bbl. and the Nienhagen field 9,340,870 bbl. Table 1 gives statistics of German production since 1928, arranged both by fields and by oil provinces. Fig. 1 demonstrates the production of the various German fields since 1890. New Fields Discovered During 1935 five new fields came into production. The first of these, the Moelme-Hoheneggelsen field near Hanover, was opened up in April. This region has been sporadically drilled for oil since 1882, but not until 1935 was production on a commercial scale obtained. The oil comes from Mesozoic sandstones on the flanks of a shallow salt plug. Also during April, oil was found in commercial quantities in the Rhine valley at Forst, near Bruchsal. Tertiary and Mesozoic sandstones cut by faults of the Rhine Graben form the reservoir structures in this area. In July a wildcat well drilled on the Fallstein structure, a broad Triassic anticline near Halberstadt, came in as a producer from Permian (Zechstein) dolomite. In September commercial oil mas found at Gifhorn, near Braunschweig, in Wealden sandstones associated with a shallow, geophysically discovered salt plug. During the same month production was obtained at Heide, in Holstein, from the Permian Rotlie-gendes formation, in a structural high on which oil seepages have been known for years. Drilling Activities Published information indicates that during 1935 drilling totaled 574,000 ft., as compared with 436,000 ft. in 1934; 233,000 ft. in 1933 and 151,000 ft. in 1932. The German Government is subsidizing wildcat

Jan 1, 1936

By Walter Kauenhowen

Germany's crude oil production during 1935 totaled 3,007,711 bbl., an increase of 36.6 per cent over the 2,202,214 bbl. produced in 1934. The Nienhagen-Haenigsen field furnished 77 per cent of the total 1935 production. Cumulative production figures for Germany's two most important oil fields, Wietze and Nienhagen, show that during the period from 1872 to the close of 1935 the Wietze field produced 13,325,536 bbl. and the Nienhagen field 9,340,870 bbl. Table 1 gives statistics of German production since 1928, arranged both by fields and by oil provinces. Fig. 1 demonstrates the production of the various German fields since 1890. New Fields Discovered During 1935 five new fields came into production. The first of these, the Moelme-Hoheneggelsen field near Hanover, was opened up in April. This region has been sporadically drilled for oil since 1882, but not until 1935 was production on a commercial scale obtained. The oil comes from Mesozoic sandstones on the flanks of a shallow salt plug. Also during April, oil was found in commercial quantities in the Rhine valley at Forst, near Bruchsal. Tertiary and Mesozoic sandstones cut by faults of the Rhine Graben form the reservoir structures in this area. In July a wildcat well drilled on the Fallstein structure, a broad Triassic anticline near Halberstadt, came in as a producer from Permian (Zechstein) dolomite. In September commercial oil mas found at Gifhorn, near Braunschweig, in Wealden sandstones associated with a shallow, geophysically discovered salt plug. During the same month production was obtained at Heide, in Holstein, from the Permian Rotlie-gendes formation, in a structural high on which oil seepages have been known for years. Drilling Activities Published information indicates that during 1935 drilling totaled 574,000 ft., as compared with 436,000 ft. in 1934; 233,000 ft. in 1933 and 151,000 ft. in 1932. The German Government is subsidizing wildcat

Jan 1, 1936

By R. E. Caffrey, S. K. Tung

This paper reports some of tile results obtained from the vapor-phase reaction of a volatile metal halide with a hydrogen and carbon dioxide mixture in an epitaxial-deposition chamber. Tile oxides deposited were silicon di oxide, aluminum oxide, mix-12tves of silicon di oxide and aluminum oxide, and titanium oxide. Tile deposited silicon di oxide was transparent and amorphous and had a density and index of refraction similar to that of thermally grown silica. The vote of etching was determined. The thickness uniformily of the oxide was found to he related to the aerodynamics of the system employed for deposition. A clear silicon di oxide layer was found to be dependent upon the quality of the surface prior- to aside deposition. The process parameters affecting the vale 0f deposition were studied. The deposited aluminum oxide was transparent, holy-cl-ysttrlliile, and possessed remarkable resistance to hydrofluoric acids. By measurements it has been shown that the deposited aluminum oxide is both insulating and continuous. ThE cleanness of an epitaxial silicon surface both immediately after growth and during device processing is thought to be one of the major factors contributing to the electrical properties of a final device. The advantage of protecting an epitaxial silicon wafer surface with an oxide grown immediately following epitaxial deposition is obvious. The successive growth of silicon and silicon diox- ide in epitaxial apparatus was studied by Steinmaier and loem.' They formed silicon dioxide films on a silicon substrate by adding water vapor to the silicon tetrachloride-hydrogen mixture in an epitaxial system. They also showed that, when a gaseous mixture of carbon dioxide and hydrogen is injected, water is formed only at elevated temperatures. Thus the reaction of water vapor and silicon tetra-: chloride will be limited to a relatively small reaction zone near the substrate. This paper reports some results of oxide films obtained from a vapor-phase reaction of a volatile metal halide with a hydrogen and carbon dioxide mixture in an epitaxial-deposition chamber. EXPERIMENTAL APPARATUS The system employed for the oxide deposition is a modification of a vertical system used to produce high-resistivity silicon layers by the hydrogen reduction of silicon tetrachloride.' The modification shown schematically in Fig. 1 consisted of an additional carbon dioxide gas stream which entered the reaction chamber with a hydrogen stream saturated with metal halide vapor and a diluting hydrogen stream. Silicon dioxide layers made from a mixture of silicon tetrachloride, hydrogen, and carbon dioxide gases will be discussed first. EXPERIMENTAL RESULTS 1) Factors Affecting the Rate of Oxidation. An epitaxial silicon layer was deposited by the hydrogen reduction of silicon tetrachloride on an n-type,

Jan 1, 1965

By C. S. Smith, Chih-Chung Wang

TURNBULL and his collaborators1,2 have developed the theory of homogeneous nucleation as applied, inter alia, to solidification of liquid metals. Vonnegut³ and Turnbull4 have shown that if a liquid metal is subdivided into small droplets a vast majority of them will undercool very considerably before solidification, generally to as low as about 0.8 of the freezing temperature on the absolute scale. The nuclei effective at small degrees of supercooling in bulk metal seem to be internal or surface heterogeneities, relatively small in number. If the metal is subdivided, those droplets that happen to contain such nuclei will solidify at a temperature not greatly below the true freezing point, but only a small part of the whole volume will be affected and the majority of the drops will under-cool to the much lower temperature at which homo- geneous nucleation occurs as a result of fluctuations. It occurred to one of the authors that an appropriate subdivision to give effective freedom from random nuclei is produced during the solidification of many alloys that contain a minor amount of a phase of low melting point, and that one might then expect marked undercooling of the distributed phase. Experimental: The alloys selected for initial study were copper with minor amounts of lead and bismuth, and aluminum with tin. In all these alloys, the major component freezes at a temperature not much below that of the pure metal, and there is little further change in constitution on cooling until the lower melting point constituent freezes in an almost pure state. Cooling curves were taken using the controlled heat flow method permitting approximate specific heats to be obtained. Chromel-alumel thermocouples were used, with the standard emf tables, since extreme precision was not needed. The crucible (3/4 in. id, 5/16 in. wall) was made of B & W K-20 insulating brick. It held about 10 cc of the alloy being investigated. The cooling rate was 2.5" to 2.9°C per min under a controlled temperature difference of 20°. Approximate specific heats were computed from the inverse rate curves together with data from a blank run and from a standard run with a copper cylinder of known heat capacity. The alloys for investigation were made from high-purity metals (99.99+pct) and cast into graphite molds. The castings were machined to fit the crucible and to provide a hole for the inner thermocouple. Cooling curves were taken after heating to a temperature about 50" above the melting point of the minor, lower melting-point, constituent. Results The lead phase in an alloy of copper with 5 pct lead did not undercool more than 3" below the melting point of lead (327°C) either as cast or after annealing to produce a new dispersion of the liquid phase. A copper-zinc-lead alloy with 23.75 pct zinc and 5 pct lead undercooled more but showed no thermal effect below 319°C. A cast alloy of copper with 5 pct bismuth undercooled to 249°C (M.P. bismuth 27l °C), but once solidification started it was completed at the same temperature. This was anticipated, since the bismuth forms a nearly continuous phase between the grains of copper, and a solid crystal nucleated anywhere would rapidly* con- sume the entire network of liquid, unless the physical continuity of the liquid were broken through volume changes, inadequate fluidity, or gas evolution. Similar arguments apply in the case of copper-lead alloys, where the lead-rich liquid forms a network along grain edges, though not grain faces. In both cases there would be a few isolated particles

Jan 1, 1951

By James T. B. Ives

The variety of copper-ore to which these notes refer is cornparatively rare, and, so far as I am aware, has not been recorded hitherto as occurring in Ontario. Moreover, the rocks of this locality differ so much in nature and mode of occurrence from the orebearing rocks of the western United States, that a description of them may be interesting. A line drawn upon a map of the region of the great lakes from the mouth of the Severn river at the Southern end of Georgian Bay, following the Canadian shore northwestward, and leaving Manitoulin island to the south, will describe the boundary between the Archaean rocks lying north of it and the Silurian rocks southward.

Jan 1, 1890

By R. S. Kinasevich, D. D. Crabtree, D. W. Fuerstenau, T. P. Meloy, A. L. Mular

This paper presents details of the concept that size reduction in comminution machines takes place by three mechanisms; namely impact, abrasion, and chipping grinding. Experimental evidence is presented to show that each of these comminution mechanisms produces particles of a characteristic size distribution. The actual product from a comminution device has been postulated to be the result of a composite of these three types of mechanisms. Composite curves are demonstrated for a material following the Gaudin-Schuhmann, Gaudin-Meloy, and Rosin-Rammler size distributions. About forty years ago, Gaudin1 showed that grinding may be considered a combination of impact and attrition. Since that time, major efforts have been devoted to studies, both experimental and theoretical, of impact and compression fracture, while attrition has been almost wholly neglected, at least quantitatively. A significant attempt to distinguish between attrition and impact grinding is the work of Tanaka2 in Japan. By means of an instrumented abrasion grinder and a drop weight device, he determined coefficients relating the increase in surface area of various materials to the energy expended by the two methods of comminution. He showed that physical properties of a material determine its response to attrition and impact grinding. By extending his ideas to ball milling, he concluded that to a large extent the basic comminution process in a ball mill is due to the impact of falling media. Because Tanaka used a mass of particles in his drop weight device, however, he did not obtain pure impact size reduction. The purpose of this paper is to define basic mechanisms of size reduction, to verify that each has a characteristic and meaningful distribution curve, and to show how a combination of these mechanisms results in a size distribution very like that produced by grinding mills. DEFINITION OF COMMINUTION MECHANISMS The product from a grinding device will be considered to be the sum of the contributions resulting from the action of three basic mechanisms of size reduction which operate in a ball and rod mill. These are impact grinding and two forms of attrition, namely abrasion grinding and chipping grinding. Each is defined below. Impact Grinding: If a straight line is obtained when the cumulative weight fraction finer than a given size is plotted on log-log paper as a function of that size, the slope of the line is defined as the distribution modulus. A number of investigators 3,4,5 have shown that impact fracture of single specimens of different composition and shape results in a distribution of daughter particles that exhibit a distribution modulus of unity. This has also been true for materials broken in slow compression. Moreover, under slow compression or impact fracture conditions, theoretical distribution equations6*' which approximate the Gaudin-Schuhmann distribution when the distribution modulus is close to unity agree reasonably well with the experimentally obtained products. If one now considers a comminution process where many impact or compression fracture events are taking place, then any rational summation of the individual events yields, in the finer size range, a Gaudin-Schuhmann distribution whose distribution modulus is also unity. If the size distribution of the product from a mill has a distribution modulus of unity, it is implied that particles are fractured in a manner which results in a comminution event having a distribution like that obtained for the breakage of single specimens. These impact events would occur when a particle is smashed between balls or between a ball and the mill liner. Attrition, on the other hand, is that form of grinding which cannot be called impact grinding, and comprises both abrasion and chipping grinding. Abrasion Grinding: Abrasion is a form of surface wear resulting when particles rub against each other or against balls or the mill liner of a tumbling mill, somewhat like a piece of wood being rubbed over a piece of sandpaper. The surface wears at a more or

Jan 1, 1964

By C. Feng, C. Elbaum

Knoop hardness measurements were carried out on large grains of iodide titanium containing different amounts of oxygen. For each oxygen content the hardness is recorded ainingas a function of the crystal orientation and of the angle 4 between the indenter diagonal and the projection of the C (hexad) axis in the surface. The results can be expressed by the following relation; hardness = n-k cos 2ø, where n and k are constants for a given oxygen content and crystal surface orientation. A NISOTROPY of hardness is a well-known phe-nomenon and has been reported for many metals.1-3 At the present time, however, such information is not available in the literature for titanium. Consequently, a systematic study of the simultaneous effects of oxygen content and crystallographic orientation on the hardness of titanium was undertaken in this laboratory. Evaluations of oxygen content in titanium are frequently carried out through hardness tests. Although such procedures may be justified in small grain specimens, the results of the present investigation indicate that the anisotropy of hardness should be taken into account in the case of coarsegrained specimens as well as in the case of pronounced preferred orientation. Materials and Experimental Procedures Iodide titanium, 99.99 pet pure and containing of the order of 0.002 wt pet O, was used throughout this investigation. The metal was arc melted in an argon atmosphere and cold rolled into strips 1/16 in. thick. These strips were subsequently recrystal-lized and strain annealed in vacuum (10" mm Hg or better) at 850°C in order to produce crystals varying in diameter from 10 to 25 mm. Oxygen was introduced into selected large crystals by heating at 700°C in an atmosphere of pure oxygen under an observed pressure of approximately 50 mm Hg. Each sample was subsequently annealed in vacuum at 850°C for 100 hr, in order to homogenize the oxygen content throughout the specimen. It was found that longer annealing was not necessary, for no change of surface hardness in a given direction was detected after prolonged annealing. The oxygen content was determined by the difference in weight of the specimens before and after the oxidation-annealing cycle. The accuracy of oxygen determination is within ±0.1 mg in samples weighing 0.5 to 1 g. A vacuum fusion analysis of oxygen was performed on several samples and gave results in good agreement with the ones obtained by the weight change. It should be emphasized that expected weight losses through evaporation of the metal in vacuum at 850°C' are many orders of magnitude lower than the precision of these measurements. Following the annealing treatment, both oxidized and unoxidized crystals were carefully polished. All detectable traces of surface cold working were removed by repeated polishing and etching. Laue back reflection X-ray patterns were taken for each crystal for the purpose of determining the orientation and ascertaining the absence of substructures detectable by this method. Hardness measurements, using a 1 kg load, were subsequently carried out on a Tukon hardness tester equipped with a Knoop indenter. The Knoop indenter was used throughout this work because indentations obtained by means of a Vickers indenter are considerably distorted due to the anisotropy of the elastic constants in titanium. Such distortions are much less pronounced in the case of Knoop indentations, although for some orientations a cer-

Jan 1, 1959

By J. S. Levine

A series of four displacement experiments has been run in a large alundum core. Flow potential distribution in each liquid phase was measured continuously through oil-wet and water-wet capillary barriers, using a null-point pressure balance, and saturated distribution was determined from electrical resistivity measurements. A method has been devised for calculating the effective (and relative) permeability to each phase at any time and at any point in the flow system for the transient displacement process. Relative permeability points have been calculated and average curves drawn for oil displacing water and water displacing oil. The values of dynamic capillary pressure have also been determined. Data have been substituted into the generalized Buckley-Leverett fractional flow equation and a comparison between actual and theoretical breakthrough recoveries is shown. Displacement experiments have been performed in the laboratory for many years in an effort to determine the effect of a number of parameters on multiphase flow in porous materials. In the literature of petroleum technology, Wyckoff and Botset' were among the first to develop the relative permeability concept and to show experimentally that oil, gas, and water can flow simultaneously through a porous medium in a precise way governed by certain fluid properties, by the relative saturation of each fluid, and by characteristics of the medium itself. Somewhat later, Leverett2 and Hassler, Brunner, and Deahl11 developed some theoretical concepts of capillary behavior in porous materials. The work of Buckley and Leverett3 presented a theoretical analysis of immiscible liquid displacement based on the equation of continuity and the Darcy equation for viscous flow of each fluid. Subsequent investigators attempting to verify the Buckley-Leverett equation have, in general, deliberately neglected the capillary pressure term or have performed experiments in such a manner that it could be neglected. Terwilliger, et al4 in 1951, obtained agreement between theory and experiment for the constant rate displacement of water by gas in a long vertical sand column. Rapoport and Leas5 have investigated the

Jan 1, 1955

By R. Shuttleworth, R. Smith

A Knudsen effusion tnethod I~as been used lo measure the vapor pressure of pure iron in the temperature range 1000° to 1500°C. Neutron-irradiated , natural iron was used and the Mn'~proclzdced by the (n, p) reaction removed by evaporation at high temperature. The results can be represented by the equation: where pM - 1.088 x 107 atm and T, = 20,890°K. A value of 100.2 kcal per g- atom was obtained for AH;. THE vapor pressure of pure iron in the temperature range 1000" to 1500°C has been measured. Radioactive iron and a Knudsen cell technique were used and the Mn' produced by an (n, p) reaction removed by evaporation at high temperature. From the variation of vapor pressure with temperature values of the enthalpy and entropy of solid iron have been found. Previous workers2 used a Lang-muir method and measurements were made over a smaller temperature range than that in this work. EXPERIMENTAL The apparatus used was similar to that of Pyle and Shuttleworth, and McLellan and Shuttle worth. However, because of the higher temperatures the Knudsen cell was machined from tungsten bar and the flanged furnace tube was beryllia. Heating was by passing a high current (70 amp at 7 v for 1500°K) through a strip of tantalum foil laid across the top of the cell and through a turn of molybdenum wire around the furnace tube. This method of heating ensured that the top of the cell was slightly hotter than the base and prevented condensation and re-evaporation from the orifice. The temperature was measured by means of a pt/Pt 13 pct Rh thermocouple spot-welded to the base of the crucible. To ensure accurate temperature measurement the iron was in the form of a thin disc (0.75 cm diam by 0.075 cm) which lay on the base of the cell. The high-purity iron was irradiated in the Harwell pile for a week at a neutron flux of 1.2 X 10" neutrons per sq cm per sec. The isotopes fe'~ and Fe" are produced by (n! y) reactions but only Fe", half-life 45.1 days, is a emitter; Mn which is also a y emitter, half-life 300 days, is produced simultaneously by an (n,p) reaction.' Immediately after irradiation of natural iron the ratio of ~e" to Mn y activity was 100:l. However, manganese is very much more volatile than iron and almost all the y activity of the condensate is due to Mn'~. Thus it was essential to eliminate all the manganeses before any measurement of the vapor pressure of iron was made and this was done by preliminary heating for 20 hr at 1400°C. For each determination the iron was dissolved from the target with acid and the y activity compared to a known weight of iron. By means of a y-ray spectrometer the y-activity measurements were made at the 1.09-mev peak of the 17e5' spectrum where the background was of the order of 3 cpm. Despite the low specific activity of ~e" a mass of 10- " g of iron could be determined corresponding to a vapor pressure of about l0-'' atm. RESULTS The vapor pressures were calculated from the equation: Where m is the mass of iron effusing in a time t through an orifice of area a2, r is the radius of the target, Z is the distance from the orifice to the

Jan 1, 1965

By O. C. Ralston

Flotation is now commonly practiced in alkaline ore pulps, yet little is known regarding the action of the alkaline solutions on the ore particles beyond the fact that films of oxidized material form. We wish to chronicle our discovery of the presence of soluble reducing agents in alkaline ore pulps of the United Verde, and present some data on lime consumption. During the grinding and flotation of a pyritic ore containing small amounts of ferrous sulfate and other soluble salts, an excess of lime was added to precipitate the salts, and filtered samples of the solution were titrated with standard permanganate solution. Even in pulps of high causticity an appreciable permanganate titration was always obtained, in spite of the fact that the solutions were shown to contain little iron. Investigation of the cause brought about the discovery of several previously unsuspected compounds in flotation pulps made from pyritic ore. Not only the reducing agents present had to be identified, but also the amount of dissolved oxygen, and a survey was finally made of the free oxygen content and reducing agents of the mill pulp in the concentrating mill at Clarkdale. A great many compounds might form, caused by oxidation of pyrite or other metal sulfides or by reaction between a lime solution and pyrite. The most probable compounds considered were calcium sulfides, polysul-fides, thiosulfates, and polythionates. Later it was discovered in the literature that in alkaline pulp polythionates do not exist and if introduced are decomposed into sulfites and thiosu1fates.l Any precipitated sulfur is changed by alkali into thiosulfate and polysulfide. Sulfites and sulfides react to form thiosulfate, so that in the end it is possible to have in an alkaline solution only thiosulfate and an excess either of sulfide or sulfite. Confirmatory tests were made and it was finally established that the alkaline mill pulps made from the United Verde ore contained

Jan 1, 1930