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By Harold Markus, Arthur H. Grobe, Gerhard Derge

THE high corrosion resistance possessed by tin under most circumstances, combined with its generally satisfactory appearance and useful physical properties, has led to many and varied uses for the metal. These uses have been partly limited by the fact that tin is an expensive metal, therefore many applications have been developed in which tin has been employed in combination with lead, either by coating, as in tin-lined collapsible tubes, or by the formation of alloys containing various proportions of tin-rich and lead-rich phases, as terne plate. A detailed knowledge of the corrosion characteristics of the tin-lead couple therefore is of general interest and has become specially important at the present time, when every effort is being made to conserve tin as much as possible. The present study. has been limited to carbonate solutions with a pH range from 8.4 to 11.2 so that the results may be related to earlier work on the corrosion of tin and its alloys.1-3,6 In these papers, the effects of a number of anion and cation additions to these solutions have been observed. APPARATUS AND METHOD The electrodes for the corrosion cell were cut from rolled sheet about 1/16 in. thick. The length of all specimens was held constant at 7 in., while the width was varied from 1/2 to 2 in. These electrodes were fastened to brass electrode supports, which were attached to rubber stoppers fitting into tall-type one-liter Pyrex beakers that contained the electrolyte. The lead electrodes were prepared from Omaha pig* and the tin was rolled from a slab of Chempur.? After cutting to size, the sheets were polished with No. I emery paper and cleaned with carbon tetrachloride. The edges, back and upper parts of the specimen were coated with a synthetic lacquer, which was supplemented with beeswax for the lead electrodes. The binding posts were coated with beeswax after the electrodes had been damped. The pH of the electrolyte was controlled? by adjusting the ratio of carbonate to bicarbonate. Approximately 600 ml. of electrolyte was used in each beaker. The entire assembly was placed in an oil bath thermostatically adjusted to operate at 30°C. ± 0.10. Potentials were measured against a saturated calomel electrode connected. to the cell by an agar-agar salt bridge. The carbonate solution used in the salt bridge was the same as that used in the corrosion cell. Currents were measured with a milliam-

Jan 1, 1942

By D. Harrington

FROM 1870 to date, the coal production of Utah has been somewhat less than 85,000,000 tons. There have been at least three major disasters with total fatalities about 380; or approximately. 4.4 persons killed by mine explosions per million tons produced, a record that is decidedly bad. Even during the periods when there have been no disasters, such as the years 1914 to 1920, inclusive, the fatalities .in ordinary working ran about 5.4 per million tons produced, against 3.7 per, million tons. for the whole United States for the same years. The five-year period following the war, 1918 to 1922 inclusive, showed 4.7 fatalities per million tons, hence the fatality record in the coal mines of Utah has uniformly been in excess of the average of the coal mines of the entire country. Notwithstanding this poor record, Utah has given to the coal-mining world many excellent safety methods and practices and the Utah. coal mines in general take greater measures toward safe mining than do the coal mines of any other State; if practices and methods allowed and pursued in coal mines of other States were tried in Utah coal mines, there would be a succession of disasters. Utah's principal producing coal mines, operated by about eighteen companies and numbering less than forty, have comparatively thick seams. Very little coal under 5 ft. thick is being worked and practically none under 4 ft.; much, if not most, of the coal comes from seams in excess of 8 ft., some running as high as 30 ft. In thick seams in which coal is left on floor and roof, any dust found or made is entirely combustible. In addition, the thick seams induce the use of large capacity cars, handling which in rooms and other workings on fairly heavy grades (up to 10 or .12 per cent.) tends to cause haulage accidents. The thick seams give high ribs and roof, in which it is difficult to prevent slabs of coal or rock from dropping on workers and also difficult to keep free of gas and of coal dust. The coal is high volatile, running usually over 40 per cent and in some instances nearly to 50 per cent; hence is highly flammable. Most of the coals have very high resin content, the resin usually being in dust form, hence almost as highly flammable as black powder. At .least one-third of the mines give off methane and several give off other

Jan 8, 1925

By Emby Kaye

It is the purpose of this paper to outline briefly some of the considerations that enter into the economics of so-called recycling, the generic designation of the relatively recently developed process by which a condensate† is separated from gas-distillate gas at high pressure and the residual gas returned to the reservoir. This subject necessarily embraces not only a discussion of factors that should be considered in projecting a recycling operation, such as estimating reserves, investment and operating costs, but also a comparison of condensate with other types of petroleum. The place of condensate in its relation to the total supply of crude oil is pointed out as well as certain logical methods of product disposal. The cost of drilling wells and lease maintenance is not pertinent to this discussion because income and revenue are in this paper confined to that retained by the plant or plant operator for supplying processing facilities for the gas. Before the development of recycling a great many gas-distillate gas fields in Louisiana and Texas provided no income to their owners. When gas was sold from these reservoirs it was accompanied by irretrievable losses of condensate in the formation. The understanding of the func- tion of retrograde condensation resulted in the introduction of a new commercial petroleum recovery process for these hitherto unexploited fields and now permits the conditioning of this type of wet gas field for the sale of dry gas therefrom without waste. Some Economic Factors The study of a gas-distillate field for possible exploitation necessarily involves the critical appraisal of a number of elements, chief of which will be discussed here: (I) estimate of distillate in place, (2) estimate of distillate that can be brought to the surface, (3) available market, (4) costs. The considerations affecting the estimating of distillate reserves in place are in the main subject to the same errors as are involved in determining dry gas reserves. Determinable data including acreage, sand thickness, reservoir pressure, reservoir temperature, porosity and connate water provide the basis for calculating the volume of gas in place. Ample allowance must be made for connate water, which may occupy from 20 to 35 per cent of the pore space of the sand. The factor of supercom-pressibility is to a considerable extent nullified by the reservoir temperature. It has been considered well advised to allow this factor to serve as a cushion. With the gas reserves calculated, it remains only to assay the distillate content of the gas. Those familiar with the handling of "wet" gas at high pressure readily appreci-ate the variables in sampling gas from

Jan 1, 1942

By Grover J. Holt

A detailed description of the many variations in iron mining and transportation practice in Minnesota would require much space. Since a fairly detailed description of the practices then in use was published in the guidebook issued in connection with the meeting of the Institute on the iron ranges in 1920, and subsequent developments have been described by E. E. Hunner, M. H. Barber,2 and A. E. Anderson, J. M. Riddell and G. J. Holt,³ it will not be necessary here to do more than review the highlights of current practice. Details on any points of interest can be obtained through correspondence with the operators involved. † The iron ores of Minnesota, which have been formed through enrichment of the iron formation in which they occur, largely by the removal of silica, are usually covered by a blanket of glacial drift known locally as "surface." Surface material, including sand, clay, hardpan and boulders, makes up the greater portion of the stripping in open-pit operations. In some instances, stripping also includes taconite and paint rock," directly below the surface material and overlying the ore. Tacenite is the iron formation, a ferruginous chert with inter-bedded slate layers. :'paint rock" is a local term for oxidized slate layers inter- bedded in the iron formation, high in phosphorus, alumina and moisture. The iron ores fall into two classes: (I) direct shipping (merchantable ores or ores requiring no treatment except possibly crushing or screening to make an acceptable sized product), and (2) ores requiring beneficiation (such as sintering, drying, washing, jigging, high-density treatment, or magnetic separation in the case of magnetite). The Mesabi Range produces chiefly soft Bessemer and non-Bessemer ores. The Cuyuna Range produces mainly low-manganese brown ore and high-manganese black ores, with some iron ore. The Vermilion Range yields mainly Bessemer and non-Bessemer iron ore, with some hard or lump ore that finds use in the open hearth. Open-pit mining is limited to the Mesabi and Cuyuna Ranges but underground mining is done on all three. The choice of mining methods is determined by the relative economics of overburden-removal and shaft-mining costs. Stripping Practice Common practice has been to remove the bulk of the overburden during the winter season and to mine during the summer, In- the present emergency many operators are forced to forego the economies attained by year-round utilization of paper. and to equip for, and carry on, stripping and mining simultaneously. In the normal years or lean years to come, most properties probably will be overequipped and high depreciation charges Will have to be absorbed.

Jan 1, 1943

By P. R. Kalischer

In the production of alloys by powder metallurgical processes it is often necessary or desirable to include one or more cornponents that tend to form very stable oxides. Included in this group of metals are aluminum, manganese, magnesium, silicon, and a few others. In many cases it is not necessary for the sintered compact to have full density and the other physical characteristics of a cast alloy and in that event no undue precautions need be taken. If, however, it is required that the sintered part be entirely homogeneous, and have maximum density and physical properties, some method must be found to reduce the surface films of oxide, which are always present on the metals, and for the metals mentioned above this is always extremely difficult, if not impossible. since the production of high-density alloys is of particular interest to powder metallurgists, some experiments were undertaken to devise methods of reducing the refractory oxides. For this work, alloys of iron, nickel, and aluminum were chosen because aluminum oxide is one of the most stable oxides and because these alloys in the right compositions form excellent permanent magnets. All of the pertinent properties of the magnets could be accurately and delicately measured by density measuremerits and magnetic tests of sufficient scope to give a complete demagnetization curve. From such a curve the maximum coercive force, residual magnetism, and energy products could be obtained and compared with the same properties for a cast material. Any lack of homogeneity, density, or solid diffusion would be immediately apparent as a decrease in the magnetic properties. Nature and Removal of Surface Barriers The early work of the present investigation was based upon published processes.* In the published information it was claimed that by intimately mixing iron, nickel, and iron-aluminum alloy (50 Per cent Fe, So Per cent Al) powders, compressing such a mixture into the desired shape and size, and then sintering (heating to a temperature below the melting point of the component metals) in hydrogen at 1200°C. or higher, a sound, homogeneous article could be made having the desired physical size, shape, and strength, and good magnetic characteristics. However. this early work showed clearly that something in the powder compress was inhibiting diffusion and the process was almost entirely unworkable. In the initial phase of the investigation samples of iron powder, nickel powder, and iron-aluminum alloy powder were pressed into separate bars and sintered in hydrogen. Both the iron and nickel powders sintered

Jan 1, 1941

By F. C. Oliphant, George H. Fancher

Two samples of drilling mud from the Hastings oil field, Texas, were tested, and the solids in each were separated into small fractions of a limited range in particle size. The mineral composition of each fraction by X-ray analysis is reported, and the results are interpreted in relation to other measured quantities, such as the physical properties of the original samples and the density of the various fractions. It was found that only 7 to 8 per cent by weight of the solids was of colloidal dimensions and that neither of the samples contained montmorillonite but did contain illite. Considerable calcite was also found. These data should be useful to the geologist interested in the origin and history of sedimentary strata as well as to the petroleum engineer. Introduction The questions, What is good drilling mud? What constitutes bad drilling mud? are pertinent, because the proper use and control of drilling fluids has been a factor of great importance in the successful drilling and completion of oil wells since the days of Captain Lucas. Adequate control of the characteristics of drilling fluids has assumed greater significance comparatively recently because of the problems introduced by caving formations in deep wells, costly blowouts and impressive mud bills. Much is known about the solution of some of the problems but, despite extensive research directed toward a better understanding of the physical and chemical properties of clay suspensions, it is difficult to define precisely a drilling mud, and much more difficult to say what constitutes a good mud. It is generally believed that the smaller particles of a drilling mud greatly affect its physical properties. In fact, it is customary to blame the colloids in a mud for nearly everything that goes amiss, because colloidal properties have effects out of all usual proportion on viscosity, filtration rate and reaction to electrolytes. It is germane to know whether drilling muds possess colloids and if so, the quantity and kind. Source oF Samples Two drilling muds from the Hastings oil field, Brazoria County, Texas, were selected because it is generally agreed that in this oil field good natural muds made solely from formations penetrated by the drill can be used until the well is nearly ready for completion. Customary drilling procedure in this field is to spud in with water, set a protective string of pipe, drill to 2500 ft. and set the surface casing. Drilling is continued to 5500 ft. with no treatment of the drilling fluid other than addition of water to

Jan 1, 1943

By C. P. Mangelsdorf

The roof truss as a means of secondary or supplemental mine roof support has enjoyed increasing acceptance in recent years, particularly in bituminous coal mines. In those entries where long life is required or doubtful performance from other forms of support seems likely, trusses in many cases have provided the necessary protection for continuing operations. Although relatively expensive and time-consuming in their installation, trusses, particularly with the new resin point anchor system, appear to be justifying their higher premium. It seems inevitable that techniques and equipment for installing them within the cycle will soon be developed. The actual mechanism by which trusses contribute to the stability of a roof is, as yet, poorly understood, and it may be that more than a single mechanism is involved. There are, however, a number of useful observations which can be made concerning the structural behavior of the truss itself, based solely on the mechanics of rigid and deformable bodies. The purpose of this article is to present some of these observations, particularly relating to friction in the system. A few speculations concerning the roof must, of course, be made. From a knowledge of the structural behavior, some insight into the truss-roof interaction may be gained. The concept of the truss is quite simple. As shown in [Fig. 1], it consists of two inclined chords (usually at 45') anchored in holes drilled in the roof over the ribs. A horizontal chord is formed connecting the exposed ends of the inclined chords, either with a third piece or by bending extensions of the inclined chords until they meet in the middle. A distinction can be made between active and passive chords of a truss depending upon the manner of installation. If the inclined chords are fully grouted and the horizontal chord is merely attached to them, it may reasonably be assumed that no significant forces exist in the truss until the roof begins to work. Such would be a completely passive system. On the other hand, if the inclined chords are anchored only at their upper extremities and the horizontal chord is formed in such a way that all three chords can be pretensioned to a significant portion of their tensile strengths then the truss may be regarded as fully active. Combinations of active and passive chords are also possible. * The discussion here is confined to the fully active truss such as the Birmingham steel rod system or the Galis wire rope truss. In both cases, pretensioning is accomplished by tightening of the horizontal chord, some of which tension is transferred to the in-

Jan 1, 1981

By A. D. Smigelskas, E. O. Karenna

This is the third paper in a series on the diffusion of zinc in alpha brass.' At the time of the first paper it was accepted that diffusion in a substitutional type of solid solution depended upon an equal interchange of solute and solvent atoms across the diffusion interface (or past a given lattice reference point). Discrepancies in the size of the areas under the diffusion curves on each side of the interface, if observed, were explained on some other basis than the fact that the solute atoms might cross the diffusion interface without an equal number of solvent atoms diffusing across the interface in the opposite direction. The second paper presented evidence indicating that zinc atoms in alpha brass diffuse across the interface more rapidly in one direction than the copper atoms diffuse across the interface in the opposite direction. This phenomenon forced the interface to move in the opposite direction of the diffusion of zinc atoms to provide space for the additional zinc atoms dissolved in the alpha brass. That the interface and columnar grain structure on one side would remain intact during this mass movement was not expected; how ever, it is gratifying that they did. While the evidence was sufficiently satisfying to the author, it was decided that additional experiments were in order to prove that zinc diffuses more rapidly than copper in alpha brass. It is the purpose of this paper to present the results of these experiments. Procedure A bar of 70-30 wrought brass was selected, to avoid the relatively large volume change in going from beta to alpha brass as in the previous investigation. A bar 7 in. (18-cm.)* long and about 3/4 in. (1.9 cm.) wide was surface ground and polished with abrasive paper on plate glass to 0.4184 0.0002 in. (1.062j + 0.0005 cm.) thick. Six0.00j-in. (0.013-cm.) diameter molybdenum wires, chosen because of their very low solubility in coppcr and alpha brass, were strctched lengthwise along each of the two plane surfaces. Glass tubes placed at right angles to the wires every 1/2 in. held the wires tightly against the brass. The sample was then emersed in an acid copper sulphate plating bath and electroplated to a depth of about 0.020 in. (0.050 cm.) copper on all sides. The glass tubes were no longer necessary to hold the molybdenum wires in place and were removed. The sample was then electroplated to a depth of

Jan 1, 1947

By C. G. Dunn

Nuclei that are formed during the recrystallization of a grain following plastic deformation generally have orientations that differ from the original. This aspect of recrystallization may be described in terms of orientation changes. It was shown previously, in an investigation on recrystallization in silicon ferrite,&apos; that the observed orientation changes were highly improbable on a chance basis, and that some mechanism must be involved. Analysis showed that the data could be satisfactorily classified into the smaller of two subclasses† of the 36 third-order twin transformations. No attempt was made at that time to classify the data within the special class of 12 third-order twin transformations, although results did indicate a greater probability for some of them to occur. A classification of this type would be more valuable, of course, with more data on orientation changes per old deformed grain. The present work fulfills this condition to some degree and also extends the scope of the investigation to include the effects of original orientation and the amount of plastic deformation. The effect of original orientation is of considerable interest because of the known effects of orientation on plastic deformation, particularly with regard to degree of fragmentation and the formation of deformation bands, and because the orientations produced by deformation should influence the orientations obtained through recrystallization. Barrett and Levenson2 reported that single crystals of iron deformed in the range 82 to 97 per cent could be put into three general classes; namely, crystals in class I maintained a reasonably sharp single orientation, those in class 2 transformed into two distinct orientations, and those in class 3 changed into a large number of major and minor orientations. Something similar would be expected for silicon ferrite crystals, and verification of this for a few cases of types class I and class 2 deformation has been reported elsewhere3 for single crystals of silicon ferrite cold-rolled in the range 10 to 20 per cent. As an example of class 2 deformation, it was shown that a crystal of silicon ferrite cold-rolled in a (110) plane in a <100> direction developed two layers, or deformation bands differing in orientation. When this happens it is possible to etch away one band and leave a single structure for use in studying the orientation changes that occur during recrystallization. when preferred crystal orientations are obtained in recrystallization, it is not particularly necessary to evaluate groups of common orientation, as was done previously (ref. I, Table 6); but an

Jan 1, 1947

By E. O. Karenna, A. D. Smigelskas

This is the third paper in a series on the diffusion of zinc in alpha brass.&apos; At the time of the first paper it was accepted that diffusion in a substitutional type of solid solution depended upon an equal interchange of solute and solvent atoms across the diffusion interface (or past a given lattice reference point). Discrepancies in the size of the areas under the diffusion curves on each side of the interface, if observed, were explained on some other basis than the fact that the solute atoms might cross the diffusion interface without an equal number of solvent atoms diffusing across the interface in the opposite direction. The second paper presented evidence indicating that zinc atoms in alpha brass diffuse across the interface more rapidly in one direction than the copper atoms diffuse across the interface in the opposite direction. This phenomenon forced the interface to move in the opposite direction of the diffusion of zinc atoms to provide space for the additional zinc atoms dissolved in the alpha brass. That the interface and columnar grain structure on one side would remain intact during this mass movement was not expected; how ever, it is gratifying that they did. While the evidence was sufficiently satisfying to the author, it was decided that additional experiments were in order to prove that zinc diffuses more rapidly than copper in alpha brass. It is the purpose of this paper to present the results of these experiments. Procedure A bar of 70-30 wrought brass was selected, to avoid the relatively large volume change in going from beta to alpha brass as in the previous investigation. A bar 7 in. (18-cm.)* long and about 3/4 in. (1.9 cm.) wide was surface ground and polished with abrasive paper on plate glass to 0.4184 0.0002 in. (1.062j + 0.0005 cm.) thick. Six0.00j-in. (0.013-cm.) diameter molybdenum wires, chosen because of their very low solubility in coppcr and alpha brass, were strctched lengthwise along each of the two plane surfaces. Glass tubes placed at right angles to the wires every 1/2 in. held the wires tightly against the brass. The sample was then emersed in an acid copper sulphate plating bath and electroplated to a depth of about 0.020 in. (0.050 cm.) copper on all sides. The glass tubes were no longer necessary to hold the molybdenum wires in place and were removed. The sample was then electroplated to a depth of

Jan 1, 1947

By W. T. Bishop, G. A. Crowe

While the literature in the United States on general polarographic technique is extensive, very little appears to be directly applicable to the analysis of flotation tailings. For this reason, it seemed worth while to present a few polarographic methods of ore analysis that have been in constant use in the laboratories of the Hercules Experiment Station for the past few years. At the time of our initial investigation of the polarographic method, there was little or no mention of its specific application to flotation tailings. It was therefore necessary for us to establish suitable conditions for the analysis of our flotation tailings and to consider possible interfering constituents. The polarograph, or dropping mercury electrode, method was discovered in 1925 by J. Heyrovsky and M. Shikata,1 of the Charles University, Prague. This method has since received extensive development and the literature contains many articles on the use of the polarograph for the quantitative determination of metals as well as anions, oxygen in solution, and reducible organic compounds. Kolthoff and Lingane,² by the publication of their book, "Polarography," in 1941 did much to advance the knowledge and use of the polarograph. In chapter 25 of that book, methods for the polarographic analysis of brass, steel and iron products, alloys, and zinc ore are given. Aluminum,³ cadmium,³,4 cobalt,4 cop-per,³-9 gold,10 iron,3,11 lead,³,l2,l³ molybdenum,14 nickel,4,8,9 tin," and zinc³,4,5,7 in ores have been analyzed by the polarograph. However, most of the work on tailing samples has been published in Russian journals and translations are not yet readily available. In this paper we will describe the method that was developed and used in our laboratory for the determination of copper, zinc, and lead in flotation tailings. Principle OF the Method The polarograph is an instrument for applying a potential to a mercury pool and a dropping mercury electrode separated by a solution, and for measuring the resultant electrical current. The procedure is essentially a small-scale electrolysis, in which the voltage required to reduce or oxidize the material identifies it qualitatively and the current measures the concentration quantitatively. Different constituents in a sample may often be determined simultaneously provided they reduce at sufficiently different voltages. An example is the determination of copper and zinc in the same solution. The reduction potentials are quite far apart, as shown in Fig. I. The polarographic method is particularly useful in the range of concentration between those normally determined by spectographic and chemical methods. In

Jan 1, 1947

By G. Gutzeit

An inner complex is a cyclic chemical structure containing an inorganic cation that is bound simultaneously to several atoms in a single organic molecule; on the one hand by means of ordinary valence bonds (electron exchange), on the other hand through the action of the electric field thus created, which satisfies the so-called secondary valences. The relative positions of the salt-forming and complex-forming groups are such that most frequently a four, five, or six-membered ring results through this double attachment of the cation.1-6 The formation of inner-complex ring systems depends not only upon the nature and suitable position of the salt-forming and complex-forming groups for ring closure, but, to a great extent, also on the nature of the metallic cation entering the reaction. This selective character of chelate-forming organic compounds is one of their most interesting and most valuable properties. As a matter of fact, the largest number of their practical applications is based upon their specificity.4,7-l3 Once a chelate compound is formed, its character is definitely "organic" in nature. In other words, its properties are conditioned to a much larger degree by the carbon chains or rings than by the metallic atom. Many inner complexes are soluble in nonpolar solvents such as benzene, paraffin oil or carbon tetrachloride, while the chelate-forming reagent before closure of the metal-organic ring is water soluble. (Example: copper complex of salicyl-aldoxime&apos;) It is obvious that such particular properties as those indicated above can be utilized whenever specificity and practically complete binding of inorganic ions into an undissociable complex are required. One of the well-known applications of chelate-forming compounds has been the development of specific reagents in analytical chemistry, creation of the spot-test method,4,14-16 and the application of the same principles to the contact print method for determining minerals." Chelate-forming Compounds as Collectors In the field of flotation, where selectivity is often a quality of paramount importance for the collector, various workers have lately attempted to apply their knowledge of specific organic analytical reagents to this purpose. A. C. Vivian18 has concentrated cassiterite by using ammonium nitrosophenylhydroxyl-amine (Cupferron) C6H5NO(=NONH4). Holmanl9 has tested dimethylglyoxime for the flotation of nickel oxide minerals, while deWitt has shown in a series of systematic experiments that alpha-diox-imes were generally selective collectors for nickel ores. Taurin NH2(CH2)2S03H has been proposed for the concentration Of Oxidized lead ores.19 Diphenylthio-carbazone

Jan 1, 1947

By C. G. Dunn

Nuclei that are formed during the recrystallization of a grain following plastic deformation generally have orientations that differ from the original. This aspect of recrystallization may be described in terms of orientation changes. It was shown previously, in an investigation on recrystallization in silicon ferrite,&apos; that the observed orientation changes were highly improbable on a chance basis, and that some mechanism must be involved. Analysis showed that the data could be satisfactorily classified into the smaller of two subclasses† of the 36 third-order twin transformations. No attempt was made at that time to classify the data within the special class of 12 third-order twin transformations, although results did indicate a greater probability for some of them to occur. A classification of this type would be more valuable, of course, with more data on orientation changes per old deformed grain. The present work fulfills this condition to some degree and also extends the scope of the investigation to include the effects of original orientation and the amount of plastic deformation. The effect of original orientation is of considerable interest because of the known effects of orientation on plastic deformation, particularly with regard to degree of fragmentation and the formation of deformation bands, and because the orientations produced by deformation should influence the orientations obtained through recrystallization. Barrett and Levenson2 reported that single crystals of iron deformed in the range 82 to 97 per cent could be put into three general classes; namely, crystals in class I maintained a reasonably sharp single orientation, those in class 2 transformed into two distinct orientations, and those in class 3 changed into a large number of major and minor orientations. Something similar would be expected for silicon ferrite crystals, and verification of this for a few cases of types class I and class 2 deformation has been reported elsewhere3 for single crystals of silicon ferrite cold-rolled in the range 10 to 20 per cent. As an example of class 2 deformation, it was shown that a crystal of silicon ferrite cold-rolled in a (110) plane in a <100> direction developed two layers, or deformation bands differing in orientation. When this happens it is possible to etch away one band and leave a single structure for use in studying the orientation changes that occur during recrystallization. when preferred crystal orientations are obtained in recrystallization, it is not particularly necessary to evaluate groups of common orientation, as was done previously (ref. I, Table 6); but an

Jan 1, 1947

By G. Gutzeit

METAL-ORGANIC INNER COMPLEXES AN inner complex is a cyclic chemical structure containing an inorganic cation that is bound simultaneously to several atoms in a single organic molecule; on the one hand by means of ordinary valence bonds (electron exchange), on the other hand through the action of the electric field thus created, which satisfies the so-called secondary valences. The relative positions of the salt-forming and complex-forming groups are such that most frequently a four, five, or six-membered ring results through this double attachment of the cation.1-6 The formation of inner-complex ring systems depends not only upon the nature and suitable position of the salt-forming and complex-forming groups for ring closure, but, to a great extent, also on the nature of the metallic cation entering the reaction. This selective character of chelate-forming organic compounds is one of their most interesting and most valuable properties. As a matter of fact, the largest number of their practical applications is based upon their specificity. 4,1-13 Once a chelate compound is formed, its character is definitely "organic" in nature. In other words, its properties are conditioned to a much larger degree by the carbon chains or rings than by the metallic atom. Many inner complexes are soluble in nonpolar solvents such as benzene, paraffin oil or carbon tetrachloride, while the chelate-forming reagent before closure of the metal-organic ring is water soluble. (Example: copper complex of salicyl-aldoxime.) It is obvious that such particular properties as those indicated above can be utilized whenever specificity and practically complete binding of inorganic ions into an undissociable complex are required. One of the well-known applications of chelate-forming compounds has been the development of specific reagents in analytical chemistry,, creation of the spot-test method,4,14-16 and the application of the same principles to the contact print method for determining minerals.17 CHELATE-FORMING COMPOUNDS AS COLLECTORS In the field of flotation, where selectivity is often a quality of paramount importance for the collector, various workers have lately attempted to apply their knowledge of specific organic analytical reagents to this purpose. A. C. Vivian18 has concentrated cassiterite by using ammonium nitrosophenylhydroxylamine (Cupferron) C6H5NO(=NONH4). Holman19 has tested dimethylglyoxime for the flotation of nickel oxide minerals, while deWitt has shown in a series of systematic experiments that alpha-dioximes were generally selective collectors for nickel ores. Taurin NH2(CH2)2SO3H has been proposed for the concentration of oxidized lead ores.19 Diphenylthiocarbazone

Jan 1, 1946

By B. N. Das, J. B. Darby, P. A. Beck, Y. Shimomura

A POWDER pattern for the (Cr, Mo, Co)R-phase annealed at 1200°C was reported in 1951.1 Through the courtesy of Prof. D. P. Shoemaker of Massachusetts Institute of Technology the authors became aware of inconsistencies of this pattern with that to be expected from the structure of the R-phase, as determined by Komura, Shoemaker, and Shoemaker.&apos; In addition, Professor Shoemaker also noted that the powder pattern reported8 for the (Cr, Mo, Co)D-phase, annealed at 1300°C, agreed fairly well with that to be expected from the newly determined structure of the R-phase. In view of these findings, the previously reported powder patterns of the R-phase and of the D-phase were compared carefully. It was found that most lines in the two patterns (22 lines) were to a fair degree of accuracy related to each other by a single conversion ratio for the corresponding d spacings. The value of the conversion ratio was found to be 1.0058, so that the d spacings of the D-phase pattern previously reported were larger than the correspond- ing d spacings for the reported R-phase pattern by approximately that factor. The intensity relationships between corresponding lines in the two patterns were similar, as judged visually. The following exceptions were noted: Lines Nos. 2, 3, 19, 20, 21, 22, 23, 24 and 25 of the D-phase pattern,:&apos; all designated weak or very weak, were missing in the apparently somewhat fainter R-phase pattern used.&apos; Lines 1, 2, 3, 5, 15 and 34 (all weak or very weak), reported for the R-phase, were missing in the D-phase pattern, Table I. In view of these observations it seemed probable that the two patterns differed from each other mainly by a slight change in lattice parameters (with c/a remaining approximately constant), and that the pattern previously reported for the R-phase contained some weak extraneous lines, most likely to be attributed to impurities. In order to check the foregoing assumption, two specimens of an alloy containing 43 pct by weight of cobalt, 41 pct molybdenum, and 16 pct chromium, which was within the composition range of stability of both the D-phase at 1300°C and of the R-phase at 1200°C, were homogenized at 1200 and 1300°C, respectively, and quenched. X-ray diffraction patterns of the powders of these two specimens, obtained with CrK radiation, were compared carefully with each other and with the D-phase pattern previously

Jan 1, 1959

Discussion of the paper of W. R. Shimer and F. O. Kichline, presented at the New York Meeting, October, 1913, and printed in Bulletin No. 81, September, 1913, pp. 2361 to 2377. ALLERTON S. CUSHMAN,* Washington, D. C.:-I have been much interested in Mr. Shimer&apos;s valuable contribution. The apparent fact that the oxides of certain metals which are not reduced by hydrogen per se, are reducible when the oxides are dissolved in iron in small quantity, is brought out for the first time, and is worthy of the careful attention of investigators. The Ledebur method has been subjected to considerable criticism, owing to the alleged fact that it did not measure the oxygen combined with impurities. Personally I have found the method extremely helpful in spite of the minute quantities of oxygen with which it deals. Mr. Shinier points out that the highest oxygen he obtained by over-blowing was 0.074 per cent., while the minimum quantity in a properly finished steel was in the neighborhood of 0.02 per cent. The Ledebur method is used as a constant check on the quality of heats made in practice under my direction. In dealing with a very pure commercial iron, we should expect to find and would find difficulty in galvanizing sheets made from a heat running 0.07 per cent. oxygen. In fact, we do not like to have the oxygen rise above 0.03 per cent. I am inclined to agree with the author that excessive oxygen leaves a bath of metal in a very short time, but nevertheless I believe it takes only a very little combined oxygen to begin to make its presence felt in the pickling and galvanizing department, when sheet metal is the product manufactured. As Mr. Shimer points out, the higher the carbon, the lower the oxygen danger, and it is partly for this reason that the manufacture of carbon-free metal in the open-hearth furnace has to be so very carefully watched and controlled from the furnace through to the finished product. It is quite possible that, there is a critical temperature of dissociation between iron and oxygen, although the critical points may vary in baths of different carbon content. Unfortunately, the accurate determination of the temperature of a molten bath at the time of pouring or teeming is a very difficult matter. For a long time I have been wishing that there were some reliable data which would indicate the effect of the tem-

Jan 12, 1913

By S. F. Radtke, J. A. Snyder, R. M. Scriver

An automatic, continuous casting arc furnace employing a nonconsum-able electrode and a direct current arc has been constructed and operated successfully for titanium. A comparison of the properties of arc and induction-melted titanium indicates that where high ductility, formability, and toughness are required, arc-melted metal is preferable. BECAUSE of the reactivity of titanium metal with all known refractories and the common atmospheric gases, melting of the metal presents numerous problems. It is necessary to provide an inert atmosphere in the furnace as well as a crucible material that will not react with the molten metal, if a ductile ingot is to be produced. Two special furnaces have been developed that meet the requirements and one, the induction heated graphite furnace, has been described in some detail.&apos; Little information is available for sizable units wherein power is applied to the melt through an arc, and the dearth of technical information on such a furnace prompted this report. It has been demonstrated clearly that arc melting produces titanium metal with superior toughness, ductility, and formability. To produce titanium ingots with these properties, an automatic, continuous casting arc furnace has been developed and is described herein. The history of arc melting may be traced to 1800, when Sir Humphrey Davy2 first experimented with Volta&apos;s electric battery and found that light could be produced and an arc formed between two carbon points attached to the cell. The discovery of the arc was followed by the design and construction of an arc furnace by Napier," in 1845, for the reduction of metal oxides. In 1853, Pichou&apos; described a similar furnace, although it was not until the discovery of the dynamo in 1867 that the arc furnace could achieve commercial significance. In 1878, Siemens- esigned the first arc furnace intended for the melting of metals and by 1882 had melted steel and platinum successfully. . This was followed by Moissan&apos;s" classical work with the arc furnace in 1892. W. von Bolton,&apos; in 1905, found that the arc furnace was suited admirably for melting refractory metals. In his work with tantalum, no suitable refractories for retaining the molten metal were found to exist. Together with Otto Simpson, he developed an arc furnace with a water-cooled copper crucible in which tantalum could be melted without contamination. This technique proved eminently successful. In his paper on the preparation of ductile titanium, Krolle first described an application of the von Bolton furnace to the melting of this metal. The

Jan 1, 1952

By P. R. Kalischer

In the production of alloys by powder metallurgical processes it is often necessary or desirable to include one or more cornponents that tend to form very stable oxides. Included in this group of metals are aluminum, manganese, magnesium, silicon, and a few others. In many cases it is not necessary for the sintered compact to have full density and the other physical characteristics of a cast alloy and in that event no undue precautions need be taken. If, however, it is required that the sintered part be entirely homogeneous, and have maximum density and physical properties, some method must be found to reduce the surface films of oxide, which are always present on the metals, and for the metals mentioned above this is always extremely difficult, if not impossible. since the production of high-density alloys is of particular interest to powder metallurgists, some experiments were undertaken to devise methods of reducing the refractory oxides. For this work, alloys of iron, nickel, and aluminum were chosen because aluminum oxide is one of the most stable oxides and because these alloys in the right compositions form excellent permanent magnets. All of the pertinent properties of the magnets could be accurately and delicately measured by density measuremerits and magnetic tests of sufficient scope to give a complete demagnetization curve. From such a curve the maximum coercive force, residual magnetism, and energy products could be obtained and compared with the same properties for a cast material. Any lack of homogeneity, density, or solid diffusion would be immediately apparent as a decrease in the magnetic properties. Nature and Removal of Surface Barriers The early work of the present investigation was based upon published processes.* In the published information it was claimed that by intimately mixing iron, nickel, and iron-aluminum alloy (50 Per cent Fe, So Per cent Al) powders, compressing such a mixture into the desired shape and size, and then sintering (heating to a temperature below the melting point of the component metals) in hydrogen at 1200°C. or higher, a sound, homogeneous article could be made having the desired physical size, shape, and strength, and good magnetic characteristics. However. this early work showed clearly that something in the powder compress was inhibiting diffusion and the process was almost entirely unworkable. In the initial phase of the investigation samples of iron powder, nickel powder, and iron-aluminum alloy powder were pressed into separate bars and sintered in hydrogen. Both the iron and nickel powders sintered

Jan 1, 1941

By H. V. Winchell

It seems to me that uniformity of mining law in North America must of necessity start with uniformity in each country. I understand that the Provinces of Canada have the right to make their own individual laws and conditions, to prescribe the terms under which the prospector or the applicant for mineral titles may secure the same. That is not true of the states in the United States. In this country, the Federal Mining Law was made applicable to the public domain, which, at the time of the adoption of this Act in 1872, was chiefly west of the Missouri River; it is impossible to locate a mining claim in most of our eastern states. It is true, however, that there are certain holdover rights, mostly obsolete, arising from the fact that at the time of the formation of the Confederation of States, the land that belonged to each state became the property of the Federal Government. I am not quite correc-t in that, it was sometime after the adoption of our Constitution, I think it was 1778, but those rights were largely, by agreement, surrendered to the Federal Government; but it is a fact that the great acquisitions of territory in the West, with the single exception of Texas, were of domain that came into the possession of the Federal Government and our Federal Mining Law applies to that territory. No state has the right to (by legislative enactment) enlarge upon the rights given by the Federal Mining Law, governing the acquisition of mining claims in its territory, within its boundaries. Each state, however, may, and some of them do, limit somewhat the rights given to the prospector. For instance, the Federal Mining Law provides that a claim may be taken, staked upon the public domain, of 600 ft. in width and 1500 ft. in length. Some of the states, like South Dakota and Colorado, have at times said "that is an excessive amount of land for a single mining claim; we will therefore limit it to 300 ft. or 200 ft. in width." There is, therefore, not any direct and immediate need for uniformity of mining laws in the United States, such as there might possibly be if it were considered at all desirable upon the whole in Canada. The initiation of mining rights under the Federal Mining Act is the act of discovery of valuable mineral in place, referring now to the lode mining claims, but the same is true of the placer claim. It is true that the emphasis has never been laid upon the word valuable and that

Jan 1, 1920

By N. A. D. Parlee

THE gas-liquid metal diffusion cell technique1-3 has been used to study the diffusion of nitrogen in Fe-C alloys. The actual apparatus and technique were the same as employed by the authors to study the diffusion of hydrogen in liquid iron.&apos; The diffusion cell&apos; was formed by immersing an alumina tube in a stagnant melt contained in an alumina crucible. The tube (hereafter called absorption tube) contained nitrogen gas at 1 atm and was connected to a sensitive gas-measuring system. The change in the average concentration of nitrogen in the melt in the absorption tube was determined by measuring the rate of absorption of nitrogen in the diffusion cell. Eq. [I], 1-3 derived from the appropriate solution of Fick&apos;s second law, was used to examine the data and to calculate chemical diffusion coefficients (D) in situations where the absorption appeared to be controlled by diffusion in the liquid: where V is the stp volume in cu cm, d is the diffusion cell diameter in cm, p, is the density of the melt in g per cu cm, pg is the stp density of nitrogen in g per cu cm, C, is expressed in wt pct, D is in sq cm per sec, and t is in min. According to Eq. [I], a plot of v vs vt should yield a straight line passing through the origin if absorption is controlled by diffusion in the liquid. The slope of this line could be used to determine the value of D under appropriate conditions. As discussed in earlier reports,1,2 the initial thermal expansion of the gas upon immersing the absorption tube distorts the line in the initial stages of a diffusion experiment. However, this is not a serious problem since the slope of V vs 6 plots can be determined from the data points obtained after the initial expansion ceases. The volumes reported on the data plot presented here represent absorption after this thermal expansion ceased. Several preliminary diffusion experiments were attempted with melts of pure iron and with Fe-C alloys containing up to 0.6 pct C. In these cases, no or very little absorption was observed. The only data obtained were for an Fe-C melt which was in addition thoroughly deoxidized by successive hydrogen and vacuum-degassing treatments. These treatments introduced an appreciable amount of aluminum into the melt and reduced its omgen content. The original charge material for this melt contained 0.23 pct s and approximately 0.001 pct &. After repeated hydrogen and vacuum-degassing treatments two diffusion experiments were performed. The analysis of the melt

Jan 1, 1968