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By John W. Bell

In the introduction to an excellent pamphlet, John Gross' makes the following statements: Although marked progress has been made along mechanical lines, the theory and conception of underlying principles have not advanced so rapidly. This lack of advance in theory may be attributed to the unfortunate situation resulting from the controversy as to whether the Rittinger or Kick law is applicable to crushing. Many pages of the technical literature are burdened with theoretical discussions in favor of one or the other of these laws, which have tended to cloud rather than to clear the atmosphere. Realizing the situation, the Milling Committee of the American Institute of Mining and Metallurgical Engineers, through its secretary, E. A. Hersam, studied the milling industry and, because of the apparently hopeless lack of agreement in the Kick versus Rittinger dispute (5, 13, 14, 0, i8, 19, 21, 22, 23. 24, 30. 34), concluded that a foundation for the theory of crushing was of primary importance. The numbers in the paragraph quoted refer to papers listed by Mr. Gross in his Bibliography on Crushing and Grinding.1 One is obliged to infer that these papers show "hopeless lack of agreement in the Kick versus Rittinger dispute." No. 22 is a paper by Arthur O. Gates2 and No. 23 is one by the writer.3 Employing the subject matter contained in papers Nos. 22 and 23 2,3 the writer will show that their authors formulated identical conclusions, based solely on experimental evidence. Exactly the same defect in the Stadler hypothesis was described in each of the two papers, although entirely different experimental methods were employed in uncovering it. Both of the authors, independently, formulated the conclusion that Rittinger's was a true hypothesis and Stadler's false. The evidence in a third paper4 will be employed to prove that Stadler's hypothesis, when examined experimentally, is worthless. STADLER'S HYPOTHESIS WORTHLESS It is the writer's opinion that the evidence available in 1915 and the corroborating evidence in 1916 was amply sufficient to eliminate the need for any further consideration of Stadler's hypothesis. Certainly the evidence produced in 1918 dealt this hypothesis its coup de grace. It follows, therefore, that in the year 1918 there was only one credible hypothesis left-the Rittinger hypothesis. Gates' Opinion What information is available in Mr. Gates' paper?2 His conclusions are not consecutively summarized, none the less they are perfectly clear. On page 876, Gates says, and it is a very significant utterance: But my results show, among other things, that many more of Stadler's energy units are obtained per foot-pound-applied in coarse than in fine crushing. This suggests a doubt as to the correctness of his unit, since one would expect a foot-pound-applied to produce the same number of "energy units," whether the feed and resulting product were coarse or fine. When Rittinger's theory is applied, the number of mesh-tons (my unit of surface produced) is

Jan 1, 1942

By D. V. Carter, C. Williams

During 1943 five oil fields and two gas-condensate fields were discovered in the East and East Central Texas district. The New Hope field, discovered by Tide Water-Seaboard in Franklin County, is the most important oil discovery since the Hawkins field in 1940. At the close of the year two oil sands were producing and two additional oil sands were being tested. The gas-condensate fields of Appleby in Nacog-doches County and the Stewards Mill field in Freestone County had only one producing well each. The Carthage field was extended 3 miles north and 4 miles west. Another well that was testing at the year end indicated a probable eastward extension of several miles. The Quitman field, in Wood County, was the most active from the standpoint of drilling operations. Approximately 48 wells were complcted during the year. The second and third most active fields were Hawkins field, Wood County, and Kildare field, Cass County, respectively. Wartime restrictions of material, together with manpower shortage and Federal spacing regulations, reduced the number of oil and gas-well completions from 265 in I942 to 171 in 1943. This represents a drop of 35 percent, or approximately 1/3, enough to replace the 531 producing wells abandoned in the district during the year. No changes were made in the price of crude oil in the district in 1943. The district produced 177,652,940 bbl. of condensate and oil during 1943. This represents an increase of approximately 11 per cent compared with the previous year. The East Texas field, which is the largest and most important field in the district, had an annual production of 128,568,647 bbl. of oil, which is approximately 6.5 per cent more than the previous year, and represents 72 per cent of the district's production of condensate and oil for the year. The district had an estimated basic daily allowable of approximately 509,000 bbl. of oil on Dec. 31, 1943. The entire district produced approximately 30 pcr cent of the state's production for the year 1943. The Hawkins field, Wood County, was operated 271 days during the year and with an average daily production of approximately 52,488 bbl. for the year. This field, which is the second largest in the district, produced 14,224,164 bbl, of oil during the year. Changes in annual production in certain fields in the district can be attributed to their ability to produce at higher rates, the demand, and transportation facilities in the war effort. The East Texas field showed an over-all decrease in reservoir pressure of 8.30 lb. during the year. Indications were that through the first quarter of 1944 the return of salt water to the reservoir was having a beneficial effect. It is hoped that, as more and more water is returned to the reser-

Jan 1, 1944

By Kenneth M. Bravinder, Jonathan E. Koogle, Dean H. Sheldon

The solution of subsurface geological problems requires an analysis of vertical and horizontal dimensional relationships. For many, the ability to visualize structures in three dimensions is not easily acquired, and for areas where the structural conditions are complicated by faulting the need arises for illustrative models. This has led to the many forms of peg models, in which the usual course of construction includes a peg for the well bore, and the suspension of strings from peg to peg to illustrate the formation correlation between wells, thus developing the usual folds and flexures. Such models proved unsatisfactory for the analysis of fault problems. Consideration was then given to the use of transparent materials. A model of the Dominguez oil field was constructed in 1935, which consisted of a series of glass panels irom well to well on which the formations were shown in color. This model, though serving its purpose at the time, proved to be impractical from the standpoints of cost, breakage hazard, and extreme difficulty in maintenance. The cost of materials was estimated to be approxi-mately $300, and the construction required the services of one man for a period of from 10 to 12 months. Maintenance after actual construction was an additional expense. Consideration was then given to the use of celluloid, and aiter some experimental work it was found that the advantages in its use were: (I) a short construction time, (2) ease of handling the material, (3) sec-tions are easily reworked, (4) low cost. Construction It would be of little value to recount here the difficulties encountered in the building of the first celluloid model. The conclusions drawn, however, suggest the following pro-cedure for those who contemplate the construction of such a model: 1. Determilzatiolz of the Scale.—Accurate geological interpretation requires the use of the same scale horizontally and vertically. It should be emphasized that the limited size of the celluloid sheets (20 by 48 in. maximum dimensions), the area to be studied, the maximum depths to be plotted, and area of possible future development are the controlling factors in adopting a scale to he used. 2. Construction of the Base.—A satisfac-tory base may be constructed by using two pieces of three-ply wood separated by strips of I by 2-in. material. This type of construction prevents warping of the base. The size of the base is determined by the dimensions of the area to be studied plus 5 in. on all sides. A map of the same scale as that adopted for the model, indicating the lines of section to be used, should be fastened to the base. 3. Constructiolt of the Frame (Fig. I).—In the construction of the frame the use of %-in. 0.d. pipe welded in a box shape is suggested, with two horizontal rods on each of the four sides, top and bottom. The top rod should be at least r in. higher than the

Jan 1, 1941

By John Wulff

In a previous paper Burwell and Wulff1 have shown by electron diffraction studies that allotropic transformations can be induced in 18-8 stainless steel by polishing to a depth of about 5 X 10-5 cm. The development of a successful etching technique, which removes accountable amounts of metal from the surface without pitting and without changing the root-mean-square profile as measured with an Abbot pro-filometer, led to the application of the whole technique and material to an investigation of various mechanical methods of surface preparation, such as grinding, lapping, superfinishing and cold-rolling. Ideally suited to such a study is 18-8 of low carbon and nitrogen content. The material can be heat-treated to produce a coarse-grained single-phase structure. On cold deformation there occurs not only a reduction in grain size but, at regions of maximum stress, a change of face-centered material to body-centered material, provided the metal is worked below about 200°C. When worked between 200"about and 415°C., diffraction studies evidence a reduction in grain size without the appearance of any new body-centered ferrite. Ferrite, which can be referred also to strains induced by carbide precipitation, is evident when the material is worked at temperatures between 4150 and 800°C. Stainless steel is advantageous because the usual surface-finishing operations do not readily oxidize it to any appreciable depth. In order to produce detectable oxide films on the surface of austenitic 18-8 in a time equivalent to that required to produce, for example, a fine ground finish on 1/2 sq. in., the sample must be held in a furnace or oxygen stream above 600°C. By using longer heating times, it is possible to achieve measurable oxide films on samples , whose surface temperatures exceed only about 250°C. Experimental Procedure The apparatus, material, and technique described in the previous paper1 were employed in this investigation. Samples of 18-8, I by I cm. by 4 mm., were carefully annealed in the austenitic range to produce a coarse-grained structure. They were then quenched and pickled to remove scale, On a lapping machine of the Graton2 type, both sides of each sample were polished to a a of 1/6 a wave length of sodium D light. Thereafter they were electrolytically etched to remove at least 1 X 10-3 cm. of the surface, a depth that is well below that of any defermations induced by surface preparation. samples of this material, carefully mounted in steel holders, were then sent to various industrial organizations known for special finishing techniques. In the instrue ment shops at the Massachusetts Institute of Technology check samples were finished by the same methods, as far as they were available. Abbot profilometer3 readings Were made on all the samples, which were then carefully degreased in double distilled benzine and alcohol, dried in a hot-filtered air blast, and kept in a desiccator. SUC-

Jan 1, 1941

By Herbert H. Kellogg

Deposits of high-silica kaolinite clays occur at many places in central Pennsylvania. These white clays were formed apparently by weathering of argillaceous quartzite and limestone. Their geology, distribution and use have been reported by Leighton.1 The larger deposits have been mined from time to time, and the clay, after washing to remove coarse sand, has found use as rubber filler, foundry clay, and in white cements. In general, the clay from these deposits contains too much grit (quartz) to be useful as paper filler, and the silica content is too high to make it useful as china clay for ceramic ware. Gravity methods for the separation of quartz from these clays have failed because of the extremely fine size of the quartz grains, but by the methods of froth flotation described in this paper these sandy kaolins can be made to yield a purified kaolinite that has a chemical composition close to that of good-grade Georgia kaolins, and is free enough from grit to be used as a paper filler. As by-products of the separation, a fine (— 325-mesh) sand assaying 95.5 per cent SiO2, and a very he (—3-micron) clay are produced. The possible ceramic uses of these products are being investigated at The Pennsylvania State College. Experimental Procedure The Sample.—The clay sample used in these tests was obtained from a small mine near Tyrone, Pa. It had already been washed to remove coarse sand, and represented the finished product of this small mine and washery. Microscopic examination showed that the clay was composed almost entirely of the minerals quartz and kaolinite, and that the quartz was present mostly in particles larger than one micron, while the kaolinite particles generally were less than 20 microns in size. The kaolinite and quartz particles were physically separable by blunging the clay in water with a suitable dispersant. Preparation of Flotation Feed.—By the addition of NaOH in an amount equal to 3 lb. per ton of solids, the clay was completely dispersed in water. Flotation feed was prepared by allowing a dispersed suspension (10 per cent solids) of the clay to stand for the period of time required for a 2.5-micron particle of quartz to settle from the top of the container to the bottom. After this settling period the suspension was decanted from the settled solids. The settled solids were redispersed in water and the separation was repeated once. The two fine fractions were then combined. Thus the clay was divided into a fine and a coarse fraction by size separation at approximately 2.5 microns.* The fine fractioh was found to have a considerably lower sand content than the raw clay (Table I), and was not treated further. The coarse fraction formed the flotation feed for all the tests described in this paper. A size separation of this type can be

Jan 1, 1947

By Takeyasu Ito, Mayumi Someno, Kazuhiro Goto

SINCE the pioneering work by Kiukkola and Wagner,1 many experiments have been reported on solid electrochemistry at elevated temperatures. However, the studies have been confined to experiments under isothermal conditions. One may conceive many situations under nonisothermal conditions. With two different temperatures T1, and T2 at the two electrodes, the electromotive force, E of a Galvanic cell will be expressed by the following equation under a steady state heat transfer in solid electrolytes of zirconia-lime and thoria-lime. E = ^ $ l&-dGO2+a(T2-Ti) [1] where tO2- is the transference number of oxygen ions in the electrolyte, Go, is the chemical potential of oxygen, and a is the coefficient of the thermoelec-tromotive force due to the temperature difference. The objective of the present study was to evaluate the coefficient of the thermoelectromotive force for zirconia-lime and thoria-lime under isobaric condition. The physical meaning of this coefficient is out of the scope of the present communication. The experimental cell assembly is schematically shown in Fig. 1. The zirconia-lime electrolyte tube and thoria-lime electrolyte tube were 8.0 mm OD and 5.0 ID, from commercial sources with chemical analyses of 94.8 wt pct ZrO2, 3.85 pct CaO, 0.83 pct SiO2, 0.25 pct TiO2, and 0.05 pct Fe2O3; and 95.0 pct ThO2, 4.0 pct CaO and rare earth metal oxides, respectively. The specific gravity was 5.5 g per cu cm for zirconia-lime and 9.8 g per cu cm for thoria-lime. Original powder size before shaping and sintering the tube was several microns for both electrolytes. The distance separating the two electrodes was 4.0 or 5.0 cm. Platinum wire of 0.5 mm diam was used for the electrodes. The temperature gradient was controlled by heating one electrode with a small heating coil of nichrome wire. The temperatures at the two electrodes were measured with two calibrated Pt-13 pct Rh:Pt thermocouples, directly contacting the two platinum electrodes. The atmosphere was either air or pure oxygen. The partial pressure of oxygen in air was considered equal at the vicinities of the two electrodes, with negligibly small thermal segregation in the gas phase. The difference of the chemical potential of oxygen was controlled only by the temperature difference at the two electrodes and not by the oxygen pressure difference. The temperature ranges were 600" to 1200°C for zirconia-lime and 850" to 1200°C for thoria-lime electrolytes. Fig. 2 shows the relation of the measured electromotive force and the difference of the oxygen chemical potential at the two electrodes for zirconia-lime and thoria-lime electrolytes. The electromotive forces in the figure were measured by a *0.05 mv potentiometer. The chemical potential difference was calculated by the following equations.'

Jan 1, 1970

By John Wulff

In a previous paper Burwell and Wulff1 have shown by electron diffraction studies that allotropic transformations can be induced in 18-8 stainless steel by polishing to a depth of about 5 X 10-5 cm. The development of a successful etching technique, which removes accountable amounts of metal from the surface without pitting and without changing the root-mean-square profile as measured with an Abbot pro-filometer, led to the application of the whole technique and material to an investigation of various mechanical methods of surface preparation, such as grinding, lapping, superfinishing and cold-rolling. Ideally suited to such a study is 18-8 of low carbon and nitrogen content. The material can be heat-treated to produce a coarse-grained single-phase structure. On cold deformation there occurs not only a reduction in grain size but, at regions of maximum stress, a change of face-centered material to body-centered material, provided the metal is worked below about 200°C. When worked between 200"about and 415°C., diffraction studies evidence a reduction in grain size without the appearance of any new body-centered ferrite. Ferrite, which can be referred also to strains induced by carbide precipitation, is evident when the material is worked at temperatures between 4150 and 800°C. Stainless steel is advantageous because the usual surface-finishing operations do not readily oxidize it to any appreciable depth. In order to produce detectable oxide films on the surface of austenitic 18-8 in a time equivalent to that required to produce, for example, a fine ground finish on 1/2 sq. in., the sample must be held in a furnace or oxygen stream above 600°C. By using longer heating times, it is possible to achieve measurable oxide films on samples , whose surface temperatures exceed only about 250°C. Experimental Procedure The apparatus, material, and technique described in the previous paper1 were employed in this investigation. Samples of 18-8, I by I cm. by 4 mm., were carefully annealed in the austenitic range to produce a coarse-grained structure. They were then quenched and pickled to remove scale, On a lapping machine of the Graton2 type, both sides of each sample were polished to a a of 1/6 a wave length of sodium D light. Thereafter they were electrolytically etched to remove at least 1 X 10-3 cm. of the surface, a depth that is well below that of any defermations induced by surface preparation. samples of this material, carefully mounted in steel holders, were then sent to various industrial organizations known for special finishing techniques. In the instrue ment shops at the Massachusetts Institute of Technology check samples were finished by the same methods, as far as they were available. Abbot profilometer3 readings Were made on all the samples, which were then carefully degreased in double distilled benzine and alcohol, dried in a hot-filtered air blast, and kept in a desiccator. SUC-

Jan 1, 1941

By Herbert H. Kellogg

Deposits of high-silica kaolinite clays occur at many places in central Pennsylvania. These white clays were formed apparently by weathering of argillaceous quartzite and limestone. Their geology, distribution and use have been reported by Leighton.1 The larger deposits have been mined from time to time, and the clay, after washing to remove coarse sand, has found use as rubber filler, foundry clay, and in white cements. In general, the clay from these deposits contains too much grit (quartz) to be useful as paper filler, and the silica content is too high to make it useful as china clay for ceramic ware. Gravity methods for the separation of quartz from these clays have failed because of the extremely fine size of the quartz grains, but by the methods of froth flotation described in this paper these sandy kaolins can be made to yield a purified kaolinite that has a chemical composition close to that of good-grade Georgia kaolins, and is free enough from grit to be used as a paper filler. As by-products of the separation, a fine (— 325-mesh) sand assaying 95.5 per cent SiO2, and a very he (—3-micron) clay are produced. The possible ceramic uses of these products are being investigated at The Pennsylvania State College. Experimental Procedure The Sample.—The clay sample used in these tests was obtained from a small mine near Tyrone, Pa. It had already been washed to remove coarse sand, and represented the finished product of this small mine and washery. Microscopic examination showed that the clay was composed almost entirely of the minerals quartz and kaolinite, and that the quartz was present mostly in particles larger than one micron, while the kaolinite particles generally were less than 20 microns in size. The kaolinite and quartz particles were physically separable by blunging the clay in water with a suitable dispersant. Preparation of Flotation Feed.—By the addition of NaOH in an amount equal to 3 lb. per ton of solids, the clay was completely dispersed in water. Flotation feed was prepared by allowing a dispersed suspension (10 per cent solids) of the clay to stand for the period of time required for a 2.5-micron particle of quartz to settle from the top of the container to the bottom. After this settling period the suspension was decanted from the settled solids. The settled solids were redispersed in water and the separation was repeated once. The two fine fractions were then combined. Thus the clay was divided into a fine and a coarse fraction by size separation at approximately 2.5 microns.* The fine fractioh was found to have a considerably lower sand content than the raw clay (Table I), and was not treated further. The coarse fraction formed the flotation feed for all the tests described in this paper. A size separation of this type can be

Jan 1, 1947

The amount of coal used in the Colonies before the Revolutionary War was very small, and few records of it can be found, these all being in the Public Records Office in London. The exports and imports for the years 1768 to 1772, inclusive, are shown in Table 3, which apparently do not include the early shipments from the Virginia field. For the three years 1769 to 1771, the imports from Great Britain-their only source-totalled 17,943 tons, or an average of 5,981 tons per year. If the shipments from Richmond for the same period were available, this average would probably not exceed 6,800 tons per year. In Table 4 the shipments of coal from the James River ports for the period 1758 to 1769 are shown. A few of them are re-exports of coal brought from England, but the great majority are undoubtedly of coal produced in Virginia, and the movement was partly to West Indian ports but mainly to Atlantic ports from Baltimore to Portsmouth, N. H. (Piscataway). In Table 5 the data in Tables 3 and 4 are combined, the exports being deducted, and this summarizes all the available data on the amount of coal consumed in the Colonies before the separation from England. As has already been stated there has been a tremendous amount of work done in the Richmond field over a long period of time, many mines were opened and in some cases operated for years, and practically no accurate data remain or have been published to show what was done. There are undoubtedly manuscripts still remaining that will contribute to much of the knowledge of this field, and it is well worth the while of the proper state authorities to collect all the information that can be found anywhere, to enable the future development of these coal deposits to benefit by the record of what was done in the past. Table 22 shows all the methods of shipment from this field, and all of the data available about tonnages moved over each of them. The shipments by the Chesterfield and Clover Hill Railroads are largely duplicated in some of the other columns, but allowance has been made for this in the estimated totals. In addition to the difficulties experienced with similar data for the other states, these Virginia records have one peculiarly their own; it was the custom to allow 5 pecks to the bushel of coal at the pit and only 4 pecks at the docks or at vessel side. In most of the figures it is not stated to which point they apply, and a considerable error may exist due to this cause, although certainly it does not apply to all of them. The notes show the sources of the figures used, and while it is probable that the totals are lower than the actual amounts produced, the data given are the most complete that can now be assembled.

Jan 1, 1942

By Gerhard Derge

The extension of metallurgical control of steelmaking processes has always made it desirable to have some quick method for determining the oxygen content of molten steel. To meet the practical demands of the steel industry, this method must also be simple enough so that the sampling can be done by the regular furnace crew. This requirement was kept in mind continually in the work to be described. An oxygen value is required for proper control, whether it be of a rimming steel or of a fully killed steel. However, two factors have discouraged the development of such direct methods: i. The reaction C + FeO Fe + CO is rapid enough to make the correct sampling Of the bath a difficult problem. The most generally accepted means of circumventing this difficulty have been the aluminum-killed bomb test of McCutcheon and Rautiol and the aluminum-killed spoon test of Herty.2 The theory of these tests is that all of the oxygen in the iron is converted to Al2O3, which can then be determined by chemical methods. Even when simplified so that the analysis is made by a measurement of turbidity, this method is too slow to be used in routine control. Furthermore, the results obtained have never been entirely satisfactory, and some of the reasons for this will be discussed later in this paper. z. The ordinary chemical methods of analysis for oxygen in steel are not reliable. The only analysis that seems to possess sufficient dependability to be of value is vacuum fusion,3 and the apparatus and technique developed for this have been too complex and slow for routine work. Indirect Methods Indirect methods of estimating the oxygen have been resorted to in mill practice. Generally these depend upon the chemical equilibria involved. The oxygen in the bath is related to other components in the slag or metal that can be analyzed the readily. These methods have many difficulties in common. Steelmaking processes involve a complicated set of interrelated reactions, all of which tend to approach equilibrium at varying rates. The degree to which any particular equilibrium is approached is not well established. Moreover, a proper use of theoretical equilibrium constants requires a more extensive knowledge of the activities of the con- than we now have. This is well illustrated by the irregularities observed when trying to determine the oxygen in the metal by its ratio to the iron oxide in the slag. Equiliblium relations may be used mole readily if they are evaluated by plant experience, but the extent of approach to equilibrium remains an undetermined variable and lack of an entirely satisfactory mean, of determining oxygen for the calibration is felt keenly, For example, the statistical analysis of the relation between carbon and oxygen4.6 illustrates that even iia a single plant wide variations exist under llormal conditions of operation. Never. theless, this is one of the best methods now

Jan 1, 1943

By Gerhard Derge

The extension of metallurgical control of steelmaking processes has always made it desirable to have some quick method for determining the oxygen content of molten steel. To meet the practical demands of the steel industry, this method must also be simple enough so that the sampling can be done by the regular furnace crew. This requirement was kept in mind continually in the work to be described. An oxygen value is required for proper control, whether it be of a rimming steel or of a fully killed steel. However, two factors have discouraged the development of such direct methods: i. The reaction C + FeO Fe + CO is rapid enough to make the correct sampling Of the bath a difficult problem. The most generally accepted means of circumventing this difficulty have been the aluminum-killed bomb test of McCutcheon and Rautiol and the aluminum-killed spoon test of Herty.2 The theory of these tests is that all of the oxygen in the iron is converted to Al2O3, which can then be determined by chemical methods. Even when simplified so that the analysis is made by a measurement of turbidity, this method is too slow to be used in routine control. Furthermore, the results obtained have never been entirely satisfactory, and some of the reasons for this will be discussed later in this paper. z. The ordinary chemical methods of analysis for oxygen in steel are not reliable. The only analysis that seems to possess sufficient dependability to be of value is vacuum fusion,3 and the apparatus and technique developed for this have been too complex and slow for routine work. Indirect Methods Indirect methods of estimating the oxygen have been resorted to in mill practice. Generally these depend upon the chemical equilibria involved. The oxygen in the bath is related to other components in the slag or metal that can be analyzed the readily. These methods have many difficulties in common. Steelmaking processes involve a complicated set of interrelated reactions, all of which tend to approach equilibrium at varying rates. The degree to which any particular equilibrium is approached is not well established. Moreover, a proper use of theoretical equilibrium constants requires a more extensive knowledge of the activities of the con- than we now have. This is well illustrated by the irregularities observed when trying to determine the oxygen in the metal by its ratio to the iron oxide in the slag. Equiliblium relations may be used mole readily if they are evaluated by plant experience, but the extent of approach to equilibrium remains an undetermined variable and lack of an entirely satisfactory mean, of determining oxygen for the calibration is felt keenly, For example, the statistical analysis of the relation between carbon and oxygen4.6 illustrates that even iia a single plant wide variations exist under llormal conditions of operation. Never. theless, this is one of the best methods now

Jan 1, 1943

By Charles H. Moore

In the study of the properties of rutile pigments it became apparent several years ago that certain physical and optical properties could not be determined on particles of pigmentary size. Since reflected light is the dominant type which reaches the eye from small particles, the true color of pure rutile was not known. Most rutile pig-ments are acicular in habit, elongated parallel to the "c" axis. It was considered important to know the nature and tone of light transmitted, for example, by a basal plate. Further, as shown by spectrophotometric curves, there is a very strong absorption of light of 4000 A as measured on particles with random orientation. It would be interesting to see whether this absorption position varied with predetermined and selected orientations. Also, since the behavior of titanium pigments in a vehicle is important, a knowledge of the surface wettability of single crystals by various media should prove very fruitful. Finally, the optical properties of rutile are such that it should show, in a single pure crystal, greater fire and brilliance than the diamond. Mineralogists had long speculated that this would be the case and curiosity was strong to produce a single crystal large enough to cut. In light of the above, a project was initiated for the formation of single crystals of rutile. Method of Formation of Rutile Single Crystals Fortunately, purification of TiO2 produced from both titanium tetra-chloride and titanyl sulphate solutions had reached the stage where spectro-graphically pure starting material could be made. Spectrographic analysis of the feed material used in the initial experiments is compared with the present feed material in Table 1. It is apparent that the present large scale purification is approximately as good as the original experimental, small scale purification. Verneuil1 produced synthetic ruby and corundum in 1904 by the well-known flame fusion process, which today bears his name. Except for mechanical improvements the present commercial production of synthetics by flame fusion is essentially unchanged from his initial method. His burner consisted of an inner orifice through which was fed the feed material and oxygen. Surrounding this was a larger outer orifice through which was fed hydrogen at lower pressure. This arrangement consists then of a lance of oxygen burning in an atmosphere of hydrogen. The proportions of hydrogen to oxygen usually used in corundum production is about 3:1, providing there is sufficient temperature to reach the 2050.°C required for the fusion of alumina. From work done in the Titanium Division Laboratories2 and from the published work of Erlich3 it was known that rutile appears to lose oxygen near its melting point and that it would not be possible to grow single crystals in a strongly reducing environment. Consequently, in order to determine whether single crystals could be grown at all, an Airco oxygen-acetylene torch with

Jan 1, 1950

By H. W. Schadler

Single crystals of tungsten, which were grown by electron bombardment floating zone refining, were strained 2 pet in tension and bending at 298°, 77°, and 20°K to determine the modes and crystallography of the plastic deformation of these temperatures. At 77° and 20°K plastic deformation occurs by slip on systems of the type (011) [111] and by twinning on (112)-type planes. For crystals strained at 298°K, deformation occurs by slip in [111] directions on either (Oil)- or (112)-type planes. CURRENT models for the initiation of brittle fracture in crystalline materials are based on a knowledge of the details of their plastic deformation.1 Body-centered cubic tungsten exhibits brittle failure at temperatures below about 500 °K yet the modes and crystallography of its plastic deformation have not been studied below 1000°K. In 1924, Goucher2 reported that tungsten single crystals with a total impurity content of less than 0.01 wt pet deformed by slip on the (112) [111] system in the temperature range 1000° to 3000°K. He also observed (001) [010] slip in one crystal which was constrained by the presence of a large fissure. According to Barrett3 tungsten also deforms by twinning on the (112) plane in the [111] direction, but he gives no details on the tendency for twin formation or the temperature range in which twinning occurs. Therefore, as a necessary part of a study of the factors influencing the brittle fracture of tungsten, the modes and crystallography of the plastic deformation were determined at 298°, 77°, and 20°K. Tungsten single crystals, grown using the electron-bombardment zone-refining technique first described by Calverly,4 were deformed to between 1 and 2 pet plastic strain in tension and bending. The surface offset resulting from slip or twinning was observed with an optical microscope to determine the crystallography of the deformation. The existence of twins was proven by the standard polishing and etching technique; and the crystallography of dislocation motion was followed using the dislocation etchant described by Wolff.5 Some observations on the fracture characteristics of tungsten single crystals are included. EXPERIMENTAL TECHNIQUES Growth, Purity, and Perfection of the Crystals-Several years ago Calverly, Davis, and Lever4 dem-onstrated the feasibility of growing tungsten single crystals by the electron-bombardment floating zone-refining technique, and Carlson6 showed that crystals produced in this way had a high degree of purity and were ductile at room temperature. Tungsten single crystals produced by this technique in equipment similar to that described by Carlson were used in this study. The starting material, a powder metallurgy product, was obtained in the form of a swaged 1/8-in. rod from the General Electric Wire Plant in Cleveland, Ohio. The crystals were grown from this material in a vacuum of 10"4 mm of Hg by passing a molten zone 1/8 in. long down the rod twice at a speed of 3 mm per min. At this zone speed

Jan 1, 1961

By A. J. Phillips, A. A. Smith, J. S. Smart

THE preparation of a sufficient quantity of high-purity copper for extensive laboratory use in the study of impurity effects has been an integral part of a research program in progress at the Central Research Laboratory of the American Smelting and Refining Co. for the past several years. Initially the degree of purity desired was that necessary to meet two essential requirements for experimental accuracy: (I) no impurity was to be present in the copper in an amount capable of producing a detectable effect on the properties to be studied, (2) even the minor changes in properties caused by the addition of extremely small amounts of individual elements were to be measured without significant interference from contaminants. In the course of the investigation, evidence has accumulated to justify the conclusion that this copper is of exceptional purity; in fact, no impurity can be detected by any chemical method or spectrographic technique known to the authors. The present paper describes the method of production of the copper and presents some of its properties. PREPARATION OF HIGH-PURITY COPPER The elimination of impurities from commercial electrolytic copper is accomplished by a three-step purification process. The first operation consists of an electrolysis through a purified CuS04-H2SO4 electrolyte using bagged anodes, low current .density (5 amp. per sq. ft.) and low temperature (25°C. max.). The electrolyte is prepared from commercial Cu2SO4 and is purified by heating the solution and adding I gram Fe as Fe 2(S04)3 to each 100 grams dissolved copper; sufficient hydrated oxide of copper, prepared from Cu2SO4 and NaOH, is supplied to precipitate Fe(OH)3, which carries down arsenic, antimony, tin, selenium, tellurium and other minor constituents. Silver and remaining traces of lead are removed by addition of Na2S to the acidified filtrate, which is then refiltered after standing hot overnight. The cold solution is made up to 30 grams per liter Cu and 150 grams per liter H2S04 and introduced without addition agents into the electrolytic system, which consists of a double row of hard-rubber battery boxes with the inside webbing and partitions removed, arranged in seven steps of ascending height. Electrolyte is uniformly supplied to the two highest cells by glass siphons operating from a constant-level reservoir, and flows by gravity through the bank of seven cells, entering each at the bottom and leaving at the top. Glass air lifts continuously supply the returning liquid to the constant-level reservoir for recirculation. Each cell contains three 434 by 43a by I-in anodes cast from high-quality electrolytic wire bar copper, various lots of which have been used with equal success. The anodes are pinned to sheet copper hangars shaped to prevent crawl of the electrolyte to the multiple-wired bus bars-which would result in fouling of the contacts and hang inside wool flannel bags stretched over open wood frames. The deposit

Jan 1, 1941

By David B. Burrows, Rlkl Kobayashi, Norman L. Carr

The viscosity of hydrocarbon mixtures, whether in the gas or liquid phase, is a function of pressure, temperature, and phase composition. This paper presents methods for the prediction of the viscosity of the gas or less dense fluid phase over the practical range of pressure, temperature, and phase compositions encountered in surface and subsurface petroleum production operations. The correlation necessary to predict the effect of pressure on viscosities is presented in Part I. Serious discrepancies in high pressure gas viscosity data in the literature are discussed. The application of the correlation to predict absolute viscosities is discussed in Part 11. Auxiliary correlations are presented to enable calculations of viscosities from a knowledge of the pressure, temperature, and gravity of the gas phase. INTRODUCTION A knowledge of the viscosity of hydrocarbon fluids is needed to study the dynamical or flow behavior of these mixtures through pipes, porous media, or more generally wherever transport of momentum occurs in fluid motion. Since flow is predominantly in the laminar region in petroleum reservoirs, the influence of fluid viscosity on this flow is especially important. As early as 1894, Onnes1 and Onnes and de Haas' noted that the viscosities of homologs under corresponding states could be correlated. The theorem of corresponding states has been further developed and applied to the viscosity of pure, nonpolar gases under pressure by Comings, Mayland, and Egly.3 It was demonstrated that the viscosity ratio could be expressed rather closely as a function of reduced pressures and temperatures, 1.e.: µ/µ1 = f( TR2 PR) ........(1) temperature, absolute units where: TR =------------------------------ ------ critical temperature. absolute units _pressure, absolute units critical pressure, absolute units µ = viscosity of gas at reduced temperature TR and reduced pressure PR µ1 =. viscosity of gas at atmospheric pressure and at temperature TR Serious discrepancies in the viscosity of pure hydrocarbon gases at high pressures have been called to Our attention by Comings, and and Egly. They made a careful analysis of the following methods commonly used to measure gas viscosities: 1. Oscillating disc viscometer4,5 2. Rolling ball viscometer6,7 3. Capillary tube viscometer12 On the basis of their analysis of the problem and their experimental data on the viscosities of methane, ethylene, carbon dioxide, and propane, they preferentially selected data obtained by the capillary tube viscometer to develop their viscosity correlation. Since then a need has existed to verify the experimental technique of Comings, Mayland, and Egly for the determination of viscosities at high pressure; to extend the data to mixtures of hydrocarbons; and to extend the range of their correlation to include higher pressures. Using the correlation procedure of Comings, May-land, and Egly, the prediction of gas viscosities is resolved into the correlation of the effect of pressure, temperature, and composition on the viscosity of hydrocarbons and their mixtures and the prediction of viscosities of mixtures of hydrocarbons and other natural gas components at one atmosphere pressure.

Jan 1, 1955

By W. J. Parton

The efficient recovery and preparation of small sizes of anthracite called No. 4 Buckwheat (3/32 by 1/32 in.) and No. 5 Buckwheat (1/32 in. by 0), pre-sent a difficult problem to the anthracite operators. In many instances preparation of these sizes, particularly No. 5 anthracite, is extremely inefficient. In many of the older preparation plants, inadequate facilities, and often none at all, were provided as an integral part of the plant for cleaning this fine anthracite. Consequently, much of the material smaller than 3/32 in. was discarded. As the demand for these sizes increased, facilities for preparing the fine sizes were often crowded into existing structures with consequent sacrifices of capacities and efficiency. In addition to this condition, the methods of preparing the finest sizes are being developed in an attempt to improve their efficiencies. Because the demand for small sizes of anthracite still is increasing, many operators would benefit by investigating and improving the cleaning equipment employed on these sizes. The object of this paper is to de- scribe a stationary screen device from which the underflow is restricted by orifices, called a launder screen, along with operating results of several applications of this screen; a settling tank in which two classified products are produced by the installation of a cylindrical partition of smaller diameter than the original tank, one product being recovered from the small tank created by the partition and one product from the space between the inner and outer tank walls; a small pocket classifier or hydraulic trap for use in removing high ash particles from a sludge flow; the classification or segregation of sludge solids occurring in a 16 in. diam pipe flow by analysis of samples procured at different zones; and the operating results of a Fahrenwald sizer, as well as the performance of the concentrating tables handling the classified products. These simple devices were employed at the collieries of the Lehigh Navigation Coal Company Incorporated, Lansford. Pa., in order to improve preparation results on the fine sizes of anthracite. Launder Screens The launder screen is a screening and dewatering device which probably could be used advantageously in the flow diagram of many fine coal plants. Fig 1 shows that it consists of a stationary screen constructed by placing 6 in. high partitions every 6 in. along a launder. Holes are then drilled on 6-in. centers across the bottom of the launder to receive pipe bushings of the desired diameter. The screen cloth is tacked on top of the partitions. When water and solids are fed to the screen, only a small portion of the total water is removed through the orifices in each compartment so that the water in the feed is distributed evenly over the whole length of the screen. The screening action which results is very efficient because the solids are kept in a fluid condition for the full length of the screen. Blinding of the screen can be minimized by the use of screen cloth

Jan 1, 1950

By G. B. Craig, G. L. Montgomery

A simple technique has been developed which reveals glide dislocations in zone-refined aluminum as etch pits. The technique has been tested quantitatively by making dislocation counts on aluminum single crystals deformed in pure bending. The method has the advantage of being insensitive to the orientation of the surface under examination. A number of etchants which will reveal dislocations in annealed aluminum have been reported.'-' These etchants apparently depend on decoration of the dislocations by an impurity (probably iron) and cannot, therefore, be used to reveal fresh glide dislocations. In addition, it is unlikely that screw dislocations will be etched because of their small attraction for impurity atoms. Amelinckx6 has reported that glide dislocations located along slip traces can be revealed by fluo-rated aqua regia. This work indicated that dislocations themselves, irrespective of decoration by impurity atoms, are responsible for the etch pits. However, as a result of additional etching experiments, Wyon and Marchin7 concluded that dislocations alone are not sufficient to explain the localization of etch pits on slip lines in aluminum using chemical etch-pitting techniques. In addition, their results show that glide dislocations are revealed only on surfaces approximately parallel to a (100) axis and that not all slip systems are attacked. These observations have been confirmed by the present authors. The technique described in this article is insensitive to the orientation of the surface, and reveals dislocations on all glide systems. Fig. 1 shows a deformed region in the neighborhood of a scratch. Dislocations can be seen along three slip traces. In the present work, single crystals of zone-refined aluminum are polished for from 2 to 5 min in a chemical polishing reagent held at 100°C, as described by Herenguel and second:' H2Sol 60 pct H3PO4 30 pct HNO3 10 pet The samples are then coated with a thin oxide film by annealing in air at 450°C for 1 hr and cooling in the furnace. After deformation, dislocation etch pits are developed by immersing the specimen in the same polishing solution which is now held at a temperature of 50°C. The formation of small hydrogen bubbles indicates that etching has occurred. The sample is immediately removed from the solution. Prolonged etching results in enlargement of the pits and, in regions of high dislocation density, the overlapping and loss of resolution of individual pits. It is the experience of the authors that contact with iron will ruinously contaminate the reagent. With careful etching, dislocations separated by half a micron can be resolved optically and the method has been shown to be sufficiently sensitive to reveal dislocations produced during the pre-easy glide region of deformation, Fig. 2. A few examples of glide-dislocation configurations, as revealed by this technique, are shown in Figs. 1 to 4.

Jan 1, 1964

By H. R. Hendricks

The ore of the Iron King mine, being very hard and having a very fine crystalline structure, presents many problems in milling that are not present in ordinary lead-zinc ores. This very fine crystallization causes much interlocking of minerals and is most prevalent between the gold and pyrite and the sphalerite and pyrite. The recovery of gold is extremely important in the economic value of the ore and therefore constitutes a large part of the metallurgical problem to be solved. All of the gold is free but it has not been observed in any of the mill products except under very high magnification. Some of the gold is tarnished, and this condition also makes recovery difficult. The gold values have been determined to be highest in association with chalcopyrite and arsenopyrite. The silver occurs mostly in association with galena and tennantite. A small amount of native silver has also been observed occasionally. The galena, being softer than the other minerals, frees much better in grinding. Some oxidation of galena is present in the ore, as the non-sulphide lead content amounts to approximately 10 pct of the total lead. Some oxidation of sphalerite is also present in the ore. Microscopic examination of the zinc concentrate shows many grains in the minus 325-mesh to be half pyrite, together with the fact that some of the zinc is marmatite, makes production of a high-grade zinc concentrate very difficult unless recovery is sacrificed. In the grinding, it has been determined that the flotation feed must be maintained at 85 pet minus 200-mesh to free the minerals sufficiently to make the best economic recoveries. Table I illustrates the effect of fine grinding. It shows that the bulk of the recovered minerals is in the minus 325-mesh size and is the part of the minerals that is more readily freed. The pyrite concentrate is not given in the table because it contains practically no minus 325-mesh. Development of Present Flowsheet and Milling Practice The first milling operation started in 1938, with a mill capacity of 140 tons daily, producing a bulk gold-silver-lead concentrate. After several stages of expansion and changes of the mill flowsheet, the mill is currently treating 380 tons of ore daily and three separate concentrates are produced. In order of their importance and value, these are: (I) lead concentrate, (2) zinc concentrate and (3) pyrite concentrate. The present average grade of mill heads is: gold 0.11 oz, silver 4.00 oz, lead 2.50 pet, zinc 7.60 pct, copper 0.22 pct, iron 22 pct and 30 pct insolubles. Specific gravity of the ore is 3.8. During the period when bulk flotation mas practiced, the flowsheet was very simple. The ore was ground fine enough to liberate as much gold, silver and lead as possible. Necessary collectors and frothers were added in sufficient quantity

Jan 1, 1949

By Walter R. Hibbard, Cyril Stanley Smith

IN 1929 one of the authors' determined the constitution of copper-silicon-manganese alloys containing over 90 per cent copper. Through a combination of circumstances the presence of the copper-silicon kappa phase was overlooked in both binary and ternary systems. In the binary system the omission has already been rectified.2,3 To establish the limits of this phase in the ternary system, the samples that had been heat-treated at the time of the original research have now been re-examined, using more careful technique. Full details of the compositions used and the temperatures and times of heat-treatment are to be found in the earlier paper .2 The etching reagent now used to distinguish the kappa phase had the following composition: hydrogen peroxide (30 vol.), 20 c.c.; water, 25 c.c.; 20 per cent potassium hydroxide solution, 5 c.c.; ammonium hydroxide (0.90 sp. gr.), 50 c.c. Table I lists the newly observed structures. In virtually every case the constituents are the same as those previously recorded, except where kappa is now shown to be present as a result of the improved etching technique. A few other changes will be noted (No. 138 at 450°C., No. 149 at 550°C., Nos. 153 and 149 at 750°C.). The change from liquid to beta in equilibrium with kappa in No. 139 at 800°C. is based upon newly heat-treated samples. The alloy is very near the solidus at 800°C. and probably there was a slight error in the old heat-treatment temperature. The isothermal phase diagrams shown in Figs. 1 to 6 were reconstructed on the basis of the new studies. The presence of manganese does not greatly change the composition limits of the kappa phase or cause the [K = a + ?] change to occur at a markedly different temperature. There is some uncertainty regarding the range of existence of beta, for alloys were not spaced very closely in composition. The proposed diagrams, however, are in accordance with the available experimental data and with the dictates of the phase rule. Theoretically necessary fields with no experimental points are delineated by dotted lines. The alpha boundaries at all temperatures are shown together in Fig. 7. This includes also some additional points on the alpha boundary at 300° and 350°C., which were obtained as a result of electrical-conductivity measurements. Two series of seven alloys with increasing manganese content but with silicon constant at 1.90 ± 0.03 per cent or 2.42 ± 0.05 per cent were cast in ingots of 3-in, diameter. These were hot-rolled, homogenized and drawn to wire, finished at 0.08-in. diameter with a 61 per cent reduction of area following annealing at 900°C. Conductivity determinations were made before and after annealing for 30 days at 300°C. or 21 days at 350°C. Figs. 8 and 9 show the change of conductivity produced by this annealing, plotted against manganese

Jan 1, 1942

By John T. Galey

An intensified search for gas, because of the shortage in the area, led to the completion of 482 wells in southwestern Pennsylvania during 1944. This number was 27 more than the number in 1943, but 118 of the wells were nonproductive. Shallow Development Oil The initial production of the 25 producers completed was slightly less than was obtained from four wells above last yearJs total. The largest well, 20 bbl., was found in the Big Injun (Miss.) sand in Morris township, Washington County, at a depth of 2085 ft. It is currently producing about 3 bbl. per day. Outside the main producing area, a well drilled in Nicholson township, Fayette County, obtained 15 bbl. per day from 1864 to 1866 ft. in the Gantz (U. Dev.) sand. The Federal subsidy of 75¢ per barrel, effective , 1, 1944, which increased to $3.40 the current pipe-line price in this area, seems to have been insufficient stimulus to materially increase drilling for oil, although more repressuring operations are contemplated. Gas The volume of initial open flow of gas developed is off slightly over 10 million cu. ft. from 36 more wells than were completed a year ago, and the average rock pressure of this new gas is more than 100 lb. less than that obtained a year ago. Apparently the best find of this year was reported in Patton township, Allegheny County, where an initial volume of over 4 million cu. ft, was encountered in the Speechley (U. Dev.) sand at a depth of from 3293 to 3303 ft. The rock pressure there, 1190 lb. per sq. in., is nearly virgin. However, this area is fairly well delimited by dry holes and docs not seem nearly so promising from the standpoint of reserves as the Armbrust area, which was discovered several Years ago. In the patton township locality another fair well with 1303 M cu. ft. open flow and 400 lb. Per 59. in. rock pressure completed in the Hundred-Foot (U. Dev.) sand at a a depth of 2125 feet. Armstrong County, as usual, leads in number of producing wells completed with lowest percentage of failures but ranks only fou th in volume of production developed. Only two wells here had more than one million cubic feet capacity, but the rock pessure was under 200 Ib. Per sq. inch. In Fayette County, where the largest portion of new gas was found, activity appears to be shifting eastward. In Luzerne township, four producers having a total combined initial open flow in excess of 10 million cu, ft, were found in the Big Injun (Miss.) sand. The best well was found also in the same area in the Speechley sand (U. Dev.) at a depth of 3460 ft. This was a 2500-M CU. ft. well in Georges township. Several wells of more than a million cubic feet capacity were found in Jackson, Washington, Wayne and Whitley townships, Greene County. None of these, however, was in a new pool.

Jan 1, 1945