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By A. R. Powell

Four, general methods have been used in the study of the decomposition of coal. The first has been directed toward the processes of coal formation, the second has been by means of microscopic studies, the third from the data of destructive distillation, and the fourth has made use of various solvents. Applying these methods to the sulfur of coal, it has been found that the organic sulfur of plant and animal life enters into the formation of coal and remains in organic combination in the final product. The inorganic sulfur is almost entirely combined as iron pyrites and marcasite. The infiltration of hydrogen-sulfide waters is doubtless a large factor in these combinations. Sulfates are found in very small quantities except where free oxygen has entered the coal strata. The mechanical mixing of detritus with the early coal material is another source of sulfur. In this case the sulfur is distributed in microscopic particles throughout the mass. In destructive distillation, a part off the sulfur comes off as hydrogen sulfide and various thiophen compounds, but this furnishes little information as to the nature of the sulfur compounds in the coal itself. The use of solvents has given valuable data concerning the sulfur compounds in coal. Fremy1 and later E. Guignet2 noted the action of alkaline solutions on coal after treatment with nitric acid and Anderson and Roberts3 showed' the presence of large quantities of organic' sulfur in the extract so obtained. In a study of the phenol extract of coal, Parr and Hadley4 found organic sulfur in the soluble organic material. These investigations proved the presence of organic sulfur in coal in addition to the inorganic forms, such as iron pyrites and sulfates. T. M. Drown5

Jan 9, 1919

By Colin MacDonald

The choices of an uranium mill flowsheet are pri- marily determined by economic feasibility with plant location and regulatory bodies playing a lesser but still important role in this determination. The host ore bodies will determine the leach pro- cess to be used for basic uranium extraction. Im- mediately following this decision, the method of leaching has to be determined. These can be: - Atmospheric leaching - Pressure leaching - In-situ leaching - Heap leaching The three previously stated criteria lay important parts in this decision. In the case of atmospheric or pressure leach and once the soluabilized uranium has been liberated from the host gang material, liquid solids separation becomes the major criteria. Three process flowsheets are available; they being: -Countercurrent decantation - Countercurrent or co-current filtration - Resin in pulp Following liquid solids separation, concentration and precipitation become the next variable choice. They being: -Solvent extraction - Fixed bed ion exchange - Fluid bed ion exchange Lastly, washing and drying of the precipitated product to remove impurities can be carried out by either filtration or centrifugation. With the exclusion of milling circuits, grinding circuits, flotation circuits, and calcining processes, we have 240 variations of the flowsheet between leaching and a dry washed precipitate. Of this total, filtration in one form or another and in single or multiple applied forms has application in 144 streams. This paper intends to discuss four (4) facets of the total flowsheet in which filtration is applied, following grinding and prior to calcining. They are: - Leached pulp liquid solid separation - Tailings dewatering - Pregnant solution clarification - Yellow cake washing and dewatering

Jan 1, 1980

By Roshan Bhappu, Laszlo Dudas, Herman Maass

Introduction Chemical and mineralogical constitution play a very important role in the processing of ores because they dictate the method, either physical or chemical, for extracting the mineral or metal. Similarly, the mineralogical nature of the ore, especially the grain size of the valuable minerals, is very important in its processing. The fineness of the grain may be such that physical separation pro- cesses may be eliminated in preference to chemical techniques. In the past, very little attention has been devoted to the geo- logical and mineralogical occurrences which may be potential sources of ores by both the geologist and mineral processing engineer. On the one hand, geologists have devoted less attention to lower grade, complex mineral deposits, and, therefore, may have inadvertently curtailed an exploration 2rogra.m. On the other hand, the metal- lurgists have neglected to study in detail the geological environ- ments and mineralization of potential ores with the view of deter- mining the critical parameter that could assist in economically processing complex submarginal deposits. In the final analysis, a chemical processing technique converts the valuable metals to a mobile state under conditions similar to those which deposited originally in the host rock. The relationship between ore-genesis and chemical processing is close when the process of mineral or metal deposition in a particular ore deposit is understood--putting the metal in solution by reversing the process of deposition is re- latively easy. For this reason, some researchers and educators have been stressing the importance of ore-genesis, geochemistry, mineral equilibria, and ionic equilibria in studying and explaining the

Jan 1, 1974

FRANCIS B. SILSBE,* Washington, D. C. (written discussion?). ?This paper is an interesting example of the -solution by the methods of metallography of what seemed at first a purely chemical problem. The authors have shown: in detail, how the well-known corrosion of spark-plug terminals is due to the dropping out of the individual crystals of the metal as it becomes surrounded by an oxide film. This corrosion is usually quite slow but in special cases may become a serious factor in limiting the life of spark plugs. There still remains the problem for the metallurgist to produce a material that will be entirely free from, this trouble. One of the most startling results of the work is. the demonstration that it affords of the deleterious effect of a mechanical stress continuously applied to material that is at the same time subject to adverse chemical or thermal conditions. The particular style of spark plug shown in the illustration, and in which serious trouble was caused by this corrosion, has the side terminals fastened at both ends and the method of assem-bling is such that a considerable initial tension is applied to the wire. It is without doubt this superimposed tension that causes the inter-crystal-line network to line up, as it were, into a few continuous and deeply penetrating transverse fissures instead of forming a great number of shallow surface cracks. This result is clearly shown both in the case of

Jan 11, 1919

By Nathaniel Arbiter

INTRODUCTION Almost seventy-five years ago problems in the recovery of sulfides from then designated slime fractions were the impetus for the development of flotation. The fall-off in recovery by gravity methods below about 200-mesh, and the shift from coarser vein deposits to more disseminated ores, particularly for copper, provided the background for flotation's rapid advances. Although the ensuing years have witnessed major improvments both in flotation reagents and in flotation machines, many problems are still with us. And since, with the exception of the unique leaching of chalcocite ores at Inspiration, flotation is still the exclusive mainstay for primary recovery of all base metal sulfides, the solution of these problems as they arise is vital to the well-being of the mining industry. Before considering the problems themselves, it will be useful to review the current status of sulfide flotation in the United States. The last comprehensive survey by the Bureau of Mines in 1975 (1) showed sulfide ore tonnages treated from 1960 to 1975 as summarized in Table 1; Table 2 gives similar data for the flotation of all non-sulfide ores. Noteworthy is the leveling off in sulfide ore tonnages in 1970-1975, with a probable further decline in the past three years, and the sharp drop in the number of plants floating sulfide ores. In contrast, the tonnages of non-sulfide ores floated, as well as the number of individual plants, has continued to increase. In spite of these trends, two-thirds of the total tonnage of the ores to which flotation is applied is still represented by sulfides. Average grades of sulfide ores in 1975 were: about 0.6 percent for copper; near 5 percent for lead; and near 3 percent for zinc. Recoveries averaged in the low 80's for copper; about 95 percent for

Jan 1, 1979

By L. A. Morley, W. T. Parry

Engineering design problems encountered by mining engineers often depend on the properties of natural granular materials such as soil, poorly consolidated sediment, fault gouge, and hydrothermally produced clay. The physical properties of such granular materials frequently are determined by the properties of silicate clays. In most mining applications, the clays are in contact with water. Swelling of clay due to water infiltration can interfere with underground support and haulage systems. Water-saturated clay on fault, fracture, and bedding planes causes slope failures in open pit mines, roof falls and heaving of weak underclays in coal mines. Water may be removed and cementing agents may be produced in clays by electrical methods. When an electrical potential gradient is applied to a charged capillary by two electrodes, water moves toward the negative electrode.1 This electrokinetic phenomena is known as electroosmosis and has been used to successfully dewater clay minerals which lack strength because of water. A consolidation effect occurs when the flow of water is accompanied by a decrease in water content. Electrochemical changes in the clay result in cementing and irreversible hardening. Theory A mathematical basis of electroosmotic phenomena is presented by Helmholtz.3 Smoluchowski5 modifies Helmholtz’ model and presents Eq. 1 to describe fluid flow velocity due to electroosmosis. For this formula, the zeta potential can be measured experimentally. The Helmholtz-Smoluchowski model is reasonably valid for clay aggregates with large pores saturated with fresh water or dilute electrolyte solutions.° An assumption used for Eq. 1 (equations are given Table 1; terms are defined in Table 2) is that the thickness of the electrical double layer surrounding the clay particles is small compared with the pore radii. Because this is generally not the case, Schmid7 presents Eq. 2. The volume charge density in the pore may be approximated from cation exchange capacity and porosity measurements. Casagrande8 offers a semi-empirical relationship (Eq. 3) for volume rate of electroosmotic flow and finds that k, is relatively constant for most clays with an average

Jan 1, 1972

By Magnus Troilius

The method of using the bromine process of determining sulphur in steel, described below, is in successful use at the Midvale Steel Works. Ten grams of drillings are weighed out and put into the 1/2-liter flask A, with long neck. The flask is connected with a wide glass tube C', which, in its turn, is connected with the absorption bulbs B, containing HCI, 1.12 specific gravity, and ahout 5 C.C. of bromine. The wide tnbe C causes the vapor to condense and flow back into the flask A during boiling. The bulbs B connect with a long glass tnbe, which may be made to carry off the bromine fumes through a hole in a window, or, better still, through a flue with powerful draught. The connections being made, 100 C.C. of boiling water are run in through the thistle tube T. The air is thus completely driven out of the flask. 100 C.C. of HC1 (about 1.19 specific gravity) are then run in. When the gas begins to run rattler slowly through B, heat is applied until boiling gradually ensues. The steel being completely dissolved, the apparatus is disconnected, and the contents of B rinsed out into a beaker of 100 C.C. capacity, into which a few C.C. of a concentrated solution of BaCI, have been previously introduced. Heat is then applied (best by means of the hot iron plate) until the bromine is completely driven off and the BaSO, has settled nicely to the bottom. The BaSO4, is then filtered off on a small

Jan 1, 1884

By T. M. Dr. Drown

(Read at the Philadelphia Meeting, February, 1878.) ZINC is, as is well known, very brittle at a temperature of about 210° C. (410° F.), and may then be readily pulverized in a mortar. By sifting it may be obtained of uniform grain. I have been accustomed to prepare products passing through 40, 60, and 80-mesh sieves, and also by bolting through a fine handkerchief. The principal analytical uses to which I have hitherto applied this material are to the reduction of iron directly from the ore by heating it with the pulverized zinc, and the reduction of ferric to ferrous compounds in solution. In the first case the pulverized ore, 0.5 gram or less, is intimately mixed with about ten times its weight of the pulverized zinc (the finer the zinc the better), in a porcelain crucible, and this mixture is covered with about the same amount of zinc. The crucible is then heated at the top of the flame of a Bunsen burner, at a dull red heat, for about ten minutes. The crucible should not be covered. When cool, the crucible, with its contents, is placed in a flask treated with hot dilute sulphuric acid, and brought quickly to a boil. The zinc and reduced iron are dissolved in a few minutes and the flask is then tightly corked and allowed to cool. When cool, the iron is directly titrated by potassium permanganate.

Jan 1, 1878

By S. W. Parr, A. R. Powell

FOUR general methods have been used in the study of the decomposition of coal. The first has been directed toward the processes of coal formation, the second has been by means of microscopic studies, the third from the data of destructive distillation, and the fourth has made use of various solvents. Applying these methods to the sulfur of coal, it has been found that the organic sulfur of plant and animal life enters into the formation of coal and remains in organic combination in the final product. The inorganic sulfur is almost entirely combined as iron pyrites and marcasite. The infiltration of hydrogen-sulfide waters is doubtless a large factor in these combinations. Sulfates are found in very small quantities except where free oxygen has entered the coal strata. The mechanical mixing of detritus with the early coal material is another source of sulfur. In this case the sulfur is distributed in microscopic particles throughout the mass. In destructive distillation, a part of the sulfur comes off as hydrogen sulfide and various thiophen compounds, but this furnishes little information as to the nature of the sulfur compounds in the coal itself. The use of solvents has given valuable data concerning the sulfur compounds in coal. Fremyl and later E. Guignet2 noted the action of alkaline solutions on coal after treatment with nitric acid and Anderson and Roberts3 showed the presence of large quantities of organic sulfur in the extract so obtained. In a study of the phenol extract of coal, Parr and Hadley4 found organic sulfur in the soluble organic material. These investigations proved the presence of organic sulfur in coal in addition to the inorganic forms, such as iron pyrites and sulfates. T. M. Drown6 attempted the analysis of the pyritic and sulfate sulfur as distinct from the organic forms by means of sodium hypobromite; no definite proof of

Jan 1, 1920

By Henry J. Williams

The main difficulty in the determination of silicon in pig-irons containing very high percentages of that element, has been due to their almost complete insolubility in acids, or mixtures of acids. The object of the present paper, which presents no new principle, is to suggest a method of determination which has repeatedly given accurate results, and which obviates completely the tediousness and uncertainty of the usual slow solution in acids. This method has been tried with pig-irons containing from 7 to 14 per cent. of combined silicon, and properly called ferro-silicons. When reduced to an impalpable powder in the agate mortar, an 11 per cent. ferro-silicon was found to resist the action of all acids, or mixtures of acids, with the exception of sulphuric acid of about 1.25 specific gravity. But the action of this acid, even during long continued heating, was very slow, 72 hours being necessary to com pletely dissolve half a gramme of the metal. The complete decomposition of 1 gramme of the metal may, on the other hand, readily he effected in a few minutes by fusion with sodium carbonate in a covered platinum crucible over a blast-lamp —the idea being to dissolve the silicon, leaving the iron in condi tion to be readily attacked by acids. The silicon dissolves as soluble sodium silicate, and metallic iron remains in a very spongy and finely divided condition. The addition of a little hot water

Jan 1, 1889

By H. L. Miaw, A. M. Gaudin, D. W. Fuerstenau

IN spite of considerable study,1-5 the nature of slime coatings in flotation is still not completely understood. However, phenomena that control flocculation and dispersion of colloidal systems are now interpreted in terms of electrical double layers."' Colloids will flocculate even though the particles carry the same charge, but when two dispersed colloids of opposite charge are mixed, flocculation ensues even more rapidly. Analogous phenomena seem responsible for slime coating on minerals in flotation systems. To shed new light on the issue it was considered desirable to devise a tool that would measure slime coatings. The usual method has been to examine photographs of presumably representative surfaces, after an intervening washing in running water. But such an examination is non-quantitative, and the changes in chemical environment represented by the washing may have removed the slime coatings that existed during flotation. To provide the possibility for a correlation with electrical double layer phenomena, the experiments were made with quartz, corundum, and iron oxide, for which electrokinetic data are available.8-12 Since the properties of the electrical double layers of these oxides depend on the pH of the solution, pH will be the most important variable. Furthermore, because the zero point of charge for silica, iron oxide, and alumina occurs at pH 3.7, 8, and 9.5, respectively, the relative charge on the slime and mineral can be changed over wide ranges. Because of its practical importance in quartz flotation, iron oxide powder was chosen as the slime. Also, its uniform composition, contrasting color, and ease of analysis make experimentation simple.

Jan 7, 1958

By Ramkrishna Agarwal

The problem of the measurement of in situ stresses in rock masses has, in recent years, become one of the prime concerns of investigators and researchers in the field of rock mechanics. Numerous instruments have been developed for that purpose and various techniques have been used to determine the absolute values of these stresses at a point.l The "stress-relief" technique has gained the widest acceptance. In its usual application it relies on one of the two following principles: (1) Measurements of the changes in a "solid inclusion" in a borehole,2 or (2) Measurements of the diametral deformation of a borehole with a free boundary." The theoretical development, in the case of the latter, is based upon an evaluation of the deformation of a circular hole in an infinite plate under the action of a uniaxial stress field. Expressions for the deformations may be obtained by using either the plain strain or the generalized plane stress theoretical approach of the classical theory of Elasticity, which assumes that the material is linearly elastic, homogeneous and isotropic. The solution for the case of a biaxial stress field is obtained by the Principal of Superposition. The circular hole becomes elliptical after deformation takes place under the action of a uniaxial or biaxial stress field applied to the plate. In the practical application of the technique, the reverse procedure is applied. A borehole is drilled in the rock and a deformation-measuring

Jan 1, 1968

By N. W. Wickersham, Ward B. Blodget, Roberts R. Boyd

The year 1926 has seen few radical changes or developments in methods of drilling and handling oil wells, but it has been a year of steady progress and development in deep drilling and production methods. Probably the outstanding development of the year was recognition by the directors of the American Petroleum Institute of the importance of natural gas in the production of oil, and the Institute directors' resolutions in December, 1926, regarding regulation of gas production with oil by state legislation. This matter is extremely important and will receive the attention of the industry in 1927. Advances in Drilling Equipment The history of the progress of deep well drilling is the solution of problems as they have confronted the operator. As the prospects for deeper production have become apparent, methods of penetrating the earth to greater depths have been devised. Rotary Equipment Improvements in the construction and in the methods of operation of rotary drilling equipment have practically caused elimination of cable tools in California for all but shallow work. The rotary drill, from 1910 when it began to be a practical factor in California, has been making steady advances, first displacing cable tools for drilling to the oil sands in proved fields and later displacing the cable-tool outfit entirely. With the perfection of machinery for taking core samples of the formation penetrated, the rotary drill has become generally used for wildcat work, continuous coring being practiced when desirable. Deep Holes The use of the rotary drill has made commercially feasible the opening of oil fields at greater depths than was considered possible with cable tools. Heavier equipment has been promptly supplied as occasion has

Jan 1, 1927

By Halbert Powers Gillette

FROM the known laws of physical chemistry I believe it can be shown that progressive mass movement of water solutions in channels has seldom been the means of ore-concentration in veins. It is my purpose in this paper to show that the force known as “osmosis” has been the principal factor in ore-formation. Convection-currents have doubtless supplemented osmosis, and the two working together have been the agencies that have gathered the scattered particles of rare minerals into the larger masses which are called ore. Osmosis is commonly thought of as a vague, feeble force that causes slow diffusion of dissolving matter through the solvent. That it is a measurable force, often of great intensity, few know, except those who are familiar with the laws of modern physical chemistry. Therefore, I may be pardoned for going briefly into the elementary mathematics of osmotic pressure and of convection-currents. The velocity of water moving through any channel is given by the Chézy formula: (1) v = c [/rs], in which r is the hydraulic mean radius; s, the slope of the channel in which gravity is the sole propulsive force; and c, the coefficient of roughness of the sides of the channel. From this formula it is evident that the smaller the channel, the smaller the velocity of water under a constant head. In rock-crevices, therefore, where the head is constant, water moves much more slowly than in large fissures, and in moving through sand or porous rock it is to an even greater degree retarded. Hence, if a mass of water-saturated sand be heated, the finer the sand-grains, the more slowly will the temperature rise at parts remote from the source of heat. Conversely, cooling is retarded the smaller the interstices or channels through which the convection-currents move. The importance of this

Jan 1, 1913

By S. J. Rothman, A. L. Harkness, L. T. Lloyd

Self-diffusion in Y uranium has been measured using U235 as the tracer isotope. The diffusion coefficient fits an Arrhenius-type equation D = 2.33 x 10 -3 exp (- 28,5000/RT) cm2/sec The values of Do and Q are unusually low and are not consistent with the values expected from theories based on a simple vacancy mechanism of diffusion. CYLINDRICAL samples, 1 cm in diam and 1/2 to 1 cm long, were prepared from high-purity uranium containing 0.0343 pct u235, Table I. The samples were water quenched from 690°C (the a-ß transformation is at 668°C) to remove preferred orientation, and annealed at 450 "C to minimize residual stresses. One end of each cylinder was polished on a 1-µ diamond lap and electropolished in a phosphoric acid solution. After a final cleaning by cathodic sputtering, a 1- to 3-µ thick layer of the tracer isotope, uranium containing 93 pct u235, was sputtered onto the sample.' To prevent contamination during the diffusion anneal, the diffusion couples were placed in a tantalum cup and covered with another piece of uranium, and the whole assembly was sealed off in an evacuated quartz tube. Annealing temperatures were constant within +2.0°C. The samples were heated and cooled slowly between room temperature and the ß-? transformation (774°C) in order to minimize distortion of the sample surface that might arise from aniso-tropic thermal expansion and density changes during phase transformations. After machining off 1/16 in. from the radius to

Jan 1, 1961

By L. H. de Wald, J. Walter Scott

The removal of lead by fire refining methods from copper of electrolytic quality is growing in importance. Particularly is this true of the refining of secondary copper and copper cathodes obtained from electrolytic cells where lead is used as the anode material, as in the electrolysis of ore-leaching solutions and foul electrolyte. When investigating the removal of small amounts of lead from molten copper in a reverberatory furnace during the refining of secondary copper of otherwise electrolytic copper quality,' it was found necessary first to know something about the distribution of the lead throughout the bath. The authors believe that it is not generally known how small amounts of lead as an impurity are distributed in a molten copper bath; that is, whether the lead is concentrated at the bottom or at the top, or whether it occurs more or less uniformly throughout the bath. The data contained in this report may help, therefore, in the development of a satisfactory fire refining method for the removal of this obstinate element from a molten copper bath. The first step was the development of a method for taking samples from various locations in the bath, at the surface and at various depths. The sampling device used, shown in Fig. 1, consisted of a 10-gram fireclay assay crucible fitted into a ring on the end of a steel rod handle of suitable length. A fireclay scorifier, 2 in. dia., with a ½-in. hole bored in the

Jan 1, 1930

By Laurance Reid

HIGH compression ratios, resulting from high injection pressures and relatively low recovery process pressures, constitute a major problem, which has confronted those engaged in gas recycling for condensate production since the beginning of that practice. Despite the numerous process developments and improvements, no entirely satisfactory solution for this prob-lem has been presented to date. Often, where the residue gas from the recovery process must be recompressed for subsurface injection, there is a substantial difference between the required injection pressure and the plant-operating pressure required to produce maximum recovery of condensate. These limitations result in high compression ratios, which, in turn, neces-sitate excessive compressor investment and operating cost. As an alternative, the operating pressure may be increased in order to lessen the compressor requirements but such a saving often is purchased at the expense of decreased condensate recovery, caused by operation at the higher pressure. Regardless of the choice, the net result is a diminished return on the capital invested in the project. The goal of future development in this field must be the complete recovery of all valuable hydrocarbon components in the reservoir fluid at pressures that, regarded as compressor suction pressure, will require minimum compressor horsepower to inject the residue gas into the formation. A com-pression ratio of 1.5 has been established as an optimum for modern compressor equipment." Therefore, in order to con-form to this optimum condition, a 3000-lb. injection pressure would require that the condensate recovery process be operated at 2000 lb. per sq. inch.

Jan 1, 1940

By B. Ladanyi, B. Hoyaux

A first requirement for assessing the safety of a rock slope, either artificial or natural, particularly if the rock behaves in an elastic-brittle manner, is a propw knowledge of the distribution of stresses within the slope and their development with time and advancement of workings. There are a uumber of different methods that can be used, in principle, for obtaining this information, such as (1) stress measurement in situ, (2) photoelasticity,1 (3) analytical methods, and (4) numerical methods. In cases where the stress distribution cannot be obtained by classical analytical methods, as in the one considered herein, either photoelasticity or numerical methods are norrnally used. However, actually, due to the rapid development of high-speed computers, increasing preference is given to the numerical methods. Among the latter, the most successful ones, to date, for determining the stress distribution in slopes have been (1) the finite difference method,2-4 (2) the lumped parameter method,5 and (3) the finite element rnethod.6 However, for determining gravity stresses in a natural rock slope, only the finite difference method has been used until now.7,8 A solution of the same problem by the finite element method will be shown here in which a particular reference is given to the development of tensile fracture zones within the slope. FINITE ELEMENT METHOD The stress analysis using the finite element method originates from an extension of the matrix analysis of structures.9 It consists in decomposing a continuous medium, assumed herein to be homogeneous and isotropic,

Jan 1, 1972

By R. Taggart, R. H. Ericksen, D. H. Polonis

MarTENSITIC a has been observed to form spontaneously from the retained ß phase during the preparation of thin foil specimens of metastable Ti-Cr alloys containing from 6.9 to 20 wt pet Cr. Similar spontaneous martensite reactions have been reported in thin foils of 0 brass' and other alloys.2 4 The absence of retained austenite in iron-based alloys has also been attributed to spontaneous decomposition during thinning.5 The present work indicates that a unique situation occurs during which the spontaneous transformation takes place when the transitional ? phase is present in the as-quenched or partially aged ß phase. Alloys containing 6.9, 7.0, 8.0, 12.0, and 20.0 wt pet Cr were prepared by the levitation melting of "io-chrome" chromium and iodide titanium. The 0.5-in.-diam ingots were vacuum-annealed at 1000oC, and wafers 0.020 in. thick were then cut from the ingots. These wafers were wrapped in molybdenum foil, encapsulated in Vycor under a reduced pressure of purified helium, and then held for 30 min at 1000°C. The specimens were quenched in water to retain the metastable high-temperature ß phase. The quenched alloys were thinned by mechanical grinding to about 0.005 in. thick, then electropolished in a solution of 300 ml methyl alcohol, 175 ml n-butyl alcohol, and 30 ml perchloric acid at a temperature of -40°C. Needle specimens 0.005 to 0.010 in. diam were taken from each ingot and heat-treated with the foil specimens. X-ray diffraction patterns indicated the structure of the 6.9, 7.0, and 8 wt pet alloys to be a

Jan 1, 1968

By Thomas M. Dr. Drown

IN experimenting in connection with Mr. P. W. Shimer (now chemist of the Thomas Iron Company, Hokendauqua, Pa.) on methods for the determination of silicon in pig iron, in order to find one which should be accurate and yet give results in a few hours, I have adopted the following procedure, which, as far as my experience goes, leaves nothing to be desired. About one gram of pig iron or steel is treated in a platinum or porcelain dish with 25 cubic centimeters of nitric acid (sp. gr. 1, 2). When action has ceased, 25 to 30 cubic centimeters of dilute sulphuric acid (one of acid and three of water) are added, and heat applied until the nitric acid is nearly or quite driven off. The heat of a water-bath is sufficient, though the process may be hastened by heating higher on a sand-bath. Water is then cautiously added (as soon as the free sulphuric acid is sufficiently cool) and the contents of the dish heated until the crystals of ferric sulphate are completely dissolved. The solution is then filtered as hot as possible, the residue washed first with hot water, then with 25 to 30 cubic centimeters of hydrochloric acid (sp. gr. 1, 12), and finally with hot water. After drying and igniting, the silica will be found to be snow-white and granular. The following are some results obtained by this method compared

Jan 1, 1879