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By Charles C. Hawes

DETERMINATION OF SILICA OXIDE iron ores usually are found in intimate association with silica and phosphorus compounds. Their quantitative separation and purification sometimes present difficult problems to the chemist. Silicic acids may represent various degrees of dehydration. They are exceedingly weak, but combine with metallic acids and form some of the most stable oxides in nature, the silicates. When iron ores are treated with hydrochloric acid, they yield practically all their iron. However, apart from rare exceptions, varying amounts of insoluble residues of silica, alumina, lime, magnesia and compounds of phosphorus, sulphur, titanium, chromium and others will be left. If the oxides of silicon, aluminum and titanium are present in small quantities, the insoluble residue is generally very small, but the presence of these oxides more usual in larger quantities. Therefore, only a special treatment can break the bond between these elements. Ore Residues Acids remove the soluble constituent of the ore, leaving the insoluble residue, which chemically is rock or gangue and must be treated accordingly. Alkali carbonates are used frequently to break up the residue, but other fluxes have also been recommended, such as a number of lead and boron salts. The introduction of these salts, which offers certain advantages, requires, however, their removal before the other constituents can be analyzed, and this elimination is sometimes difficult. Usually in quantitative analysis silicates are dissociated by fusing them in a platinum crucible with sodium carbonate, thereby forming sodium silicate, Na2SiO3, sodium aluminate, Na2A1204, sodium titanate, Na2TiOs, and carbonates of other elements. All the carbonates are soluble in hydrochloric acid, but also some silicic acid is formed that must be rendered insoluble. To this end the solution is evaporated several times, as the first evaporation still leaves as much as 5 per cent of the silica soluble. Even after a number of evaporations, minute quantities of silica may be found with the iron and alumina present. Perchloric Acid as an Agent for Dehydrating Silicic Acid Perchloric acid, HCI04, (60 per cent), has been used for years as a solvent, but few chemists have used it to dehydrate silica. It is derived from anhydrous perchloric C1207, which is most unstable and dangerous. Perchloric acid is a strong oxidizing agent, which boils at 203°C. It is more effective in rendering silica insoluble than any other known agent, and most rapid in action. After perchloric acid is added to a mixture containing silicic acid, the resultant solution is

Jan 1, 1945

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 Lucien Eaton

THE accuracy with which detachable bits can be sharpened and gauged by grinding has made possible refinements in design that cannot be attained by forging. This applies particularly to gauging, where accuracy is of the greatest importance. Gauge changes of 1/32 in., and even 1/16 in., are now feasible, whereas 1/16 -in. changes are about the limit in accuracy for forged bits. These small changes in gauge are feasible, however, only with certain fundamental principles of design. Within reasonable limits the depth to which a hole can be drilled is dependent primarily upon the loss in gauge, or diameter, of the bit. In drilling there is always a certain amount of " overdrilling "-the bouncing of the bit in the hole and its rotation wear away the walls-so that the actual diameter of the hole is greater than the diameter of the bit. The amount of this overdrilling depends upon the kind of rock being drilled, and is sometimes sufficient to permit the use of the same diameter of bit for the full depth of the hole. If, for instance, a 1 ¾ -in. diameter bit overdrills 1/32 in. in diameter, and loses 1/64 in. in gauge in drilling 2 ft. of hole, the bottom of the hole is still 1/64 in. larger than the original diameter of the bit, and a new 1 3/4-in. bit can be used to drill the next 2 ft. If, however, the overdrill is less than the loss in gauge, the next bit must be of smaller diameter. The first requisite in reducing loss of gauge in drilling is to have the points and corners of the wings of the bit cut circles of the same diameter, thus producing a reaming surface with continuous bearing on the wall of the hole. The greater the reaming surface, the less the gauge loss that is to be expected. If the reaming surface, however, is too large, it may impede the rotation of the bit through excessive friction. This principle was probably first recognized in the design of the Carr bit (Fig. 1)) a bit with a single cutting edge of wide angle, a definite reaming edge, and a large center hole. The same idea was followed in designing the double-taper cross bits, which are now standard almost everywhere Fig. 2 illustrates a typical double-taper cross bit. The taper from the point of the wing A to a little behind the corner B is 5° and from

Jan 1, 1939

By W. C. Hagel

Previous inuestigators have repovted unusually low H* and Do values for self-dzf@szon in certazn bcc metals, e.g., chromium nnd y -uvanium. It has been postulated that this is nn experimental crl -tetion for the existpnce of a four -atom ring meclzanzsm, mid there could be. zmpovtant theoretrcal Implicatlons. By utilizing a precise sectioning technique with Cr51 as the tracer, self-dzffi-lsion measurements in large grains of 99.99-pct Cr were extended from 1200° fo 1600"C. A least- squares analysis of the data yields that D 0.280 exp (-73,20U/RT) cm2 sec-'. These AH* and Do unlues are not anomalous; there is little reason to believe that n vacancy mechanism is not opevatiue. Apparent differences at lower temperatures may result from preferential diffusion along short-circuititing paths and/or sample contamination. WITH continued technological effort, chromium and chromium-base alloys should ultimately become useful high-temperature structural materials. Accurate measurements of self-diffusion coefficients in the pure metal are necessary for a quantitative understanding of sintering, grain growth, creep, and other related rate processes. However, two conflicting determinations have been reported.* Using an Since careful diffusion studies normally yield Do values ranging from 0.1 to 10 cm2 sec-l, the Paxton-Gondolf results require independent experimental corroboration before an undue amount of speculation arises to explain the apparent anomaly. As discussed by Nowick6 and clearly shown by Hoffman and Turn-bull7 for self-diffusion in silver, a low AH* and Do can arise from preferential diffusion along grain boundaries or other short-circuiting paths. The most reliable data come from high-temperature measurements where volume effects predominate. Following a precise sectioning technique developed for determining silver diffusion in the intermetallic compound AgMg8 and cation diffusion in the corundum oxide Cr2O3,9 the purpose of this study was to measure true volume diffusion in high-purity, large-grain samples at higher temperatures than considered previously. Another point of interest is the frequent proposal10-12 that chromium undergoes an allotropic transformation between 1375" and 1800°C where the diffusion data might then show a discontinuity. I EXPERIMENTAL 1) Sample Preparation. The highest purity (99.997 pet) Cr currently available is produced by reduction of chromium tri-iodide. Three pounds of the resulting crystal bar were shipped in a sealed container with a complete chemical analysis from the vendor.* In conformity with the procedure used for

Jan 1, 1962

By David V. Ragone, Richard E. Balzhiser

The liquidus uranium concentration in the U-Bi system is given by the following expression for the temperature range 400° to 800°C: No break was observed in the curve over this temperature range. The partial molar enthalpy change for uranium in the liquidus reaction, UBi2— U + 2Bi, was found to equal 12,300 cal per g mole. Copper produced a continuous decrease in the liguihs uranium concentration at 600°C. The presence of copper in the solvent was observed to affect the uranium activity coefficient according to the following expression: duced no change in the liquidus combosition below 0.6 at. pct Pd. Higher palladium concentrations sharply depressed the uranium concentration. SOLUTE behavior in molten alloys has been shown to be strongly influenced by the presence of additional species. Much attention has been given to such phenomena in iron-base systems where a number of alloying elements and/or impurities are likely to be present in small but significant quantities. Frequently, the interaction of these solutes has altered their thermodynamic behavior to the extent that reaction equilibra are appreciably influenced. Consequently, much of the information available for binary behavior must be reevaluated when additional components are likely to be present. Similar interactions can be expected to occur in bismuth-base solvents. Interest in the use of bismuth solutions of uranium as reactor fuels has stimulated investigators to explore the effect of various elements on the liquidus uranium concentration. Criticality requirements necessitate close control of the uranium concentration which, at the anticipated operating temperature of 500°C, approaches saturation. Consequently, elements which suppress the liquidus concentration could produce serious reactivity problems. Since the fuel solution is cer- tain to contain additives, such as magnesium and zirconium, for corrosion inhibition as well as small concentrations of fission products and corrosion products, a better understanding of the possible interaction phenomena is mandatory. This need stimulated experimental programs at the Brookhaven National Laboratory and elsewhere to determine precisely the liquidus uranium concentration in the bismuth-rich portion of several ternary systems. Early experimental efforts were directed toward an accurate dcmtermination of the U-Bi liquidus over the temperature range from 300' to 800°c. As shown in Fig. 1, the results to date exhibit considerable scatter. The investigations of Bareis,' Teitel,2 Greenwood,3 and Cotterill and hon4 agreed well below 700°c. Greenwood and Teitel extended their studies to higher temperatures but failed to concur in their results. A more recent study by Schweitzer and weekss at Brookhaven National Laboratory between 300' and 725°c, produced values 15 pct lower

Jan 1, 1962

By J. H. Frye, C. P. Sun

A PRIMARY substitutional solid solution is a solution that has the same crystalline structure as the solvent metal, and in which solute atoms have replaced solvent atoms at random on the host lattice. This replacement usually results in an increase in hardness as measured by conventional penetration tests. The factors controlling this hardness increase have been investigated in some detail for copper and silver aneys.1-5 It has been shown that at least, four factors are involved: (I) concentration of solute, (2) row of the periodic table from which the solute is taken, (3) increase in lattice parameter of the solvent produced by the solute, and (4) work-hardening produced by penetration of the hardness indenter.2,4 The last factor is of the utmost importance. An investigation of the available data2.4 leads to the conclusion that the solutes that produce large hardness increases in copper or silver do so principally because they increase the rate of work-hardening. Furthermore, it is doubtful whether any solute produces appreciable hardening in the absence of plastic deformation and hence work-hardening. Thus it is clear that an understanding of the effect of solutes on rate of work hardening is essential to an understanding of the hardness of solid solutions. This effect of solutes is also important in forming operations such as rolling or deep drawing. The presence of elements that confer rapid rates of work-hardening will increase power consumption and may well decrease the amount of deformation possible between anneals. This paper is the report of an investigation of the factors that control rates of work-hardening in copper and silver solid solutions. The silver and copper alloys considered are those in which all solutes are from the B subgroups or second short period of the periodic table. Experience with hardness, with structure of alloys, and with electrical conductivity has proved that results of a fundamental nature are most likely to be obtained if alloys are made up on the basis of the positions of the constituent elements in the periodic table. In previous work, Meyer analysis data on high-purity copper and silver solid solutions were obtained through careful measurements with fully calibrated equipment and these data were corrected to correspond to a standard grain size. From these corrected Meyer analysis data rates of work-hardening have now been calculated. CALCULATION OF RATES OF WORK- HARDENING The Meyer analyses, on which this study of rates of work-hardening is based, consisted in determining impression

Jan 1, 1944

By Secretary

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

Jan 1, 1886

By J. H. Frye, C. P. Sun

A Frimary substitutional solid solution is a solution that has the same crystalline structure as the solvent metal, and in which solute atoms have replaced, solvent atoms at random on the host lattice. This replacement usually results in an increase in hardness as measured by conventional penetration tests. The factors controlling this hardness increase have been investigated in some detail for copper and silver alloys.1-5 It has been shown that at least four factors are involved: (1) concentration of solute, (2) row of the periodic table from which the solute is taken, (3) increase in lattice parameter of the solvent produced by the solute, and (4) work-hardening produced by penetration of the hardness indenter.2,4 The last factor is of the utmost importance. An investigation of the available data2,4 leads to the conclusion that the solutes that produce large hardness increases in copper or silver do so principally because they increase the rate of work-hardening. Furthermore, it is doubtful whether any solute produces appreciable hardening in the absence of plastic deformation and hence work-hardening. Thus it is clear that an understanding of the effect of solutes on rate of work-hardening is essential to an understanding of the hardness of solid solutions. This effect of solutes is also important in forming operations such as rolling or deep drawing. The presence of elements that confer rapid rates of work-hardening will increase power consumption and may well decrease the amount of deformation possible between anneals. This paper is the report of an investigation of the factors that control rates of work-hardening in copper and silver solid solutions. The silver and copper alloys considered are those in which all solutes are from the B subgroups or second short period of the periodic table. Experience with hardness, with structure of alloys, and with electrical conductivity has proved that results of a fundamental nature are most likely to be obtained if alloys are made up on the basis of the positions of the constituent elements in the periodic table. In previous work, Meyer analysis data on high-purity copper and silver solid solutions were obtained through careful measurements with fully calibrated equipment and these data were corrected to correspond to a standard grain size. From these corrected Meyer analysis data rates of work-hardening have now been calculated. Calculation of Rates as Work- HARDENING The Meyer analyses, on which this study of rates of work-hardening is based, consisted in determining impression

Jan 1, 1944

By J. H. Frye, C. P. Sun

A Frimary substitutional solid solution is a solution that has the same crystalline structure as the solvent metal, and in which solute atoms have replaced, solvent atoms at random on the host lattice. This replacement usually results in an increase in hardness as measured by conventional penetration tests. The factors controlling this hardness increase have been investigated in some detail for copper and silver alloys.1-5 It has been shown that at least four factors are involved: (1) concentration of solute, (2) row of the periodic table from which the solute is taken, (3) increase in lattice parameter of the solvent produced by the solute, and (4) work-hardening produced by penetration of the hardness indenter.2,4 The last factor is of the utmost importance. An investigation of the available data2,4 leads to the conclusion that the solutes that produce large hardness increases in copper or silver do so principally because they increase the rate of work-hardening. Furthermore, it is doubtful whether any solute produces appreciable hardening in the absence of plastic deformation and hence work-hardening. Thus it is clear that an understanding of the effect of solutes on rate of work-hardening is essential to an understanding of the hardness of solid solutions. This effect of solutes is also important in forming operations such as rolling or deep drawing. The presence of elements that confer rapid rates of work-hardening will increase power consumption and may well decrease the amount of deformation possible between anneals. This paper is the report of an investigation of the factors that control rates of work-hardening in copper and silver solid solutions. The silver and copper alloys considered are those in which all solutes are from the B subgroups or second short period of the periodic table. Experience with hardness, with structure of alloys, and with electrical conductivity has proved that results of a fundamental nature are most likely to be obtained if alloys are made up on the basis of the positions of the constituent elements in the periodic table. In previous work, Meyer analysis data on high-purity copper and silver solid solutions were obtained through careful measurements with fully calibrated equipment and these data were corrected to correspond to a standard grain size. From these corrected Meyer analysis data rates of work-hardening have now been calculated. Calculation of Rates as Work- HARDENING The Meyer analyses, on which this study of rates of work-hardening is based, consisted in determining impression

Jan 1, 1944

By C. Edwin Nighman

THE following is a description of the methods used in rescuing men and extinguishing the underground fire at the Pennsylvania mine, Butte, Mont. This fire, which cost the lives of 21 men, began about 9 p.m., Feb. 14, 1916, at or near a ventilating fan on the 1,200 air-shaft station. This shaft at that time was downcast, while the main hoisting shaft was upcast. Owing to the proximity of the fire to the air shaft, the air in the latter soon became heated, and as the fan on the level was not running¬the power having been cut off shortly after the outbreak' of the fire-the aim' shaft became upcast to the 300 level. At this point a blanket of cold air from the surface caused the smoke and gases to he drawn in on that level and carried down again through the workings to the 1,200. A short time after the discovery of the fire, water was turned down the air shaft through a series of pipes around the collar of the shaft, which caused the smoke to recede, below the 300, so that within 2 hr. it was possible to search that level for the missing men. From the above it will be apparent why the air shaft was upcast instead of downcast as under normal conditions, and why men were suffocated at considerable distances from the seat of the fire. The smoke and gases that came up the main hoisting shaft did not diffuse through the workings to any extent. There are doors on all levels in the connections to the main hoisting and air shafts, but-in the confusion and running around many of these doors were left open, and this undoubtedly caused the smoke and gases to spread more rapidly than they would otherwise have done. It was necessary for most of the men on the various levels to pass close to the air shaft in going to the hoisting shaft, and when they encountered the smoke and gases in that vicinity a number turned hack and climbed down with the direction of the air currents and were then suffocated, while all those who passed through the relatively short pall of smoke to the main shaft were saved.

Jan 2, 1917

By H. Fechtig, R. H. Buck, A. G. Guy

MULTIPHASE diffusion has been studied for many years in two-component systems1,2 and many of the experimental aspects are now fairly well understood.314 Although by no means all of the problems connected with the two-component case have been solved,' attention has recently been directed to the more complex situation involving three components. The pioneer work of Clark and Rhines6 yielded a qualitative picture of the types of behavior that can occur, and Clark7 has suggested conventions for describing the various phenomena. Kirkaldy and co-workers8,9 have made quantitative studies in several ternary systems and have offered explanations of the occurrence of isolated and nonisolated precipitates. At present, however, there is no comprehensive theory for the variety of phenomena observed in ternary, multiphase diffusion. By analogy with several studies that have been made of multiphase diffusion in the binary Cu-Zn system,2'10'11 a similar exploratory study was made of Cu-Zn-Ni alloys lying along the line in the ternary diagram from the point 80 Cu-20 Ni to the zinc corner of the diagram, Fig. 1. A principal question to be answered was whether initially plane interfaces would remain plane during the course of one-dimensional diffusion. The diffusion specimens studied are described in Table I. The five separate alloys from which they were made were melted in evacuated Vycor capsules from 99.9 pct purity copper, zinc, and nickel. Since some of the alloys were too brittle to be swaged, all of the alloys were used in the cast condition. To facilitate later homogenization, the molten alloys were solidified by plunging the capsule in water. Homogenization heat treatment was done at 720°C for 20 hr. The five nominal compositions in weight percent zinc and nickel, respectively, were: 37.5, 12.5; 44.0, 11.2; 50.0, 10.0; 55.0, 9.0; 65.0, 7.0. Ln Table I the alloys are identified only by their zinc content. Sandwich-type diffusion specimens were prepared by pressure welding disk specimens, each about 3 mm high by 10 mm in diameter. Welding was done in a special threaded vise which was heated at 500°C for about an hour in an atmosphere of flowing hydrogen. A measurement of the separation of the phase interfaces was made on a polished flat on the welded specimen, and then the specimen was sealed in an evacuated capsule and given the diffusion treatment shown in Table I. The diffused specimen was sectioned longitudinally

Jan 1, 1965

By R. W. Bowers

In order to hoist the ore according to grades, stope samples are taken. Three equidistant grooves are picked across the breast at right angles to the dip of the ore, the part removed being caught in the hand and then put into a small bag. When there is broken ore in the breast, the lines are continued down the pile and a small amount taken at intervals of the length of the sampler's pick handle. The quantity of sample from each breast will be between 2 and 3 Ib. If there are two grades of ore, bessemer and non-bessemer, there are two sets of brass checks for each chute, each check stamped with the number of the chute; one set of checks has the word "bessemer" and the other "non-bessemer." Before any ore is removed from the chutes, it is the duty of one man to see that the proper set of checks is at each chute in the mine. As each motor car is loaded, a check is attached to it. When the train reaches the shaft, the sample man removes the check on the first car, notes the grade, and directs the motorman to spot it over the proper pocket. The check is then hung on a hook with the number corresponding to the chute from which the ore came. The sample man throws a short rope with a knot in the end over the car and at the point where the knot falls a standard scoopful is taken. This is placed in a large bag that hangs directly under the hook containing the checks for that particular chute. These chute samples represent a check on the grading of the various contracts and by counting the tags a check is obtained on the miner's tally of the ore going into each chute; the total of the checks represents the hoist. During the stocking season, a standard scoopful is taken from each top tram car. This sample is taken in the same way as the chute samples at the plats underground. Top-of-car Samples These samples are taken by using a rope, preferably a clothesline, knotted each 18 in. of its length, and a hammer and a scoop. The standard scoop measures 31/2 by 21/4 by 11/4 in. and holds about 1/2 Ib. of ore. The rope, as applied to the usual railroad cars at the mine, is knotted into fifteen sections. It is placed diagonally over the car from

Jan 1, 1925

By R. H. Sweetser

The Committee on Evaluation of Coal for Blast-furnace Coke reports progress in the working out of the problem of evaluation. There has been no full meeting of the Committee but there have been several conferences with two or more of the members present, and the different members have expressed themselves freely on the five points that have been under consideration since the meeting of the Committee in New York on Feb. 16, 1932. The need of a method of coal evaluation, not only of coking coals but all other kinds, is obvious. Under NRA it becomes imperative that coals of the same size from the same seam be priced according to their variations in quality, especially in reference to cleanliness in respect to freedom from extraneous ash-forming materials. In looking over the correspondence that has passed between members of our Committee, it is evident that much of the confusion and misunderstanding would disappear if we could realize that practically all of the variations in value of coal from the same seam of coal are due to variations in the amounts of extraneous materials that are contained in the coal as it passes over the scales for shipment. It is not now a question with our committee as to the differentials in value, or in prices, between different kinds of coking coals or between noncoking and coking coals; our present problem is to arrive at the method for determining the scale of values of the coal from a certain coal seam according to the increase or decrease of extraneous ash and moisture from a predetermined base line adopted for that particular coal. The five points mentioned above are the same as discussed at the meeting in February, 1932, except that the temperature for determining the moisture content has been changed from 212" F. to 221" F., at the suggestion of Dr. A. C. Fieldner. The points are: 1. It is proposed that the coal industry adopt as a base line for evaluating all coals the analysis of the coal as it passes over the neighing device that determines the tonnage of coal bought and sold. 2. It is proposed that the Committee on Evaluation of Coal for Blast-furnace Coke approve the adoption of the base line for Pittsburgh seam coal presented by F. A. Jordan at the annual meeting of A.I.M.E.

Jan 1, 1934

By E. M. Porbansky

DURING the investigation of the electrical transport properties of copper, it became necessary to prepare large single crystals of the highest obtainable purity. In an effort to meet these demands, single crystals of copper have been grown by the conventional pulling technique—as has been used for the growth of germanium and silicon crystals.' Low-temperature resistance measurements made on these crystals show that, as far as their electrical properties are concerned, they are generally of significantly higher purity than the original high-purity material. The use of these pure single crystals with very high resistance ratios has made possible the acquisition of detailed information regarding the electron energy band structure of copper2-' and has stimulated widespread effort on Fermi surface studies of a number of other pure metals. It is the purpose of this note to describe our method of preparing very pure copper crystals by the Czochralski technique. Precautions were taken to prevent contamination of the melt from the crystal growing apparatus. A new fused silica growing chamber was used to prevent possible contamination from previous groqths of other materials such as germanium, silicon, and so forth. A new high-purity graphite crucible was used to contain the melt. This crucible was baked out in a hydrogen atmosphere at -1200°C for an hour, prior to its use in crystal growth. Commercial tank helium, containing uncontrolled traces of oxygen, was used as the protective atmosphere. A trace of oxygen in the atmosphere appears to be necessary for obtaining high-purity copper single crystals. A 3/8-in-diam polycrystalline copper rod of the same purity as the melt was used as a seed. The copper rod was allowed to come in contact with the melt while rotating at 57 rpm. When an equilibrium was observed between the melt and the seed (that is, the seed neither grew nor melted), the seed was pulled away from the melt at a rate of 0.5 mils per sec. As the seed was raised, the melt temperature was slowly increased, so that the grown material diminished in diameter with increasing length. When this portion of the grown crystal was -1 in. long and the diameter reduced to less than 1/8 in., the melt was slowly cooled and the crystal was allowed to increase to - 1-1/4 in. diam as it was grown. By reducing the diameter of the crystal in this manner, the number of crystals at the liquid-solid interface was decreased until only one crystal remained. Fig. 1 shows a typical pulled copper single crystal. The purity of the starting material and the crystals was determined by the resistance ratio method: where the ratio is taken as R273ok/R4.2ok. The starting material, obtained from American Smelting and Refining Co., was the purest copper available. Most of the pulled copper crystals had much higher resistance ratios than the starting material. The highest ratio obtained to data is 8000. Table I is an example of the data obtained from some of the copper crystals. Note that Crystal No. 126 had a lower resistance ratio than its starting material and this might be due to carbon in the melt. The melt of this crystal was heated 250" to 300°C above the melting point of copper. At this temperature it was observed that copper dissolved appreciable amounts of carbon. The possible presence of carbon at the interface between the liquid and the crystal will result in reducing conditions and negate the slight oxidizing condition required for high purity as discussed below. The possible explanations of the improvement in the copper purity compared to the starting material are: improvement in crystal perfection, segregation, and oxidation of impurities. Of these, the latter seems to be most probable. A study of the etch pits in the pulled crystals showed them to have between 107 and 108 pits per sq cm. The etch procedure used was developed by Love11 and Wernick.10 The resistivity of the purest copper crystal grown was 2 x 10-10 ohm-cm at 4.2oK; from the work of H. G. vanBuren,11 the resistivity due to the dislocations would be approximately 10-l3 ohm-cm, which indicates that. the dislocations in the copper crystals would contribute relatively little to the resistivity of the crystals at this purity level. Segregation does not seem likely as the reason for purification of the material, since the resistivity of the first-to-freeze and the last-to-freeze portions are approximately the same, as was observed on Crystal No. 124. On most of the crystals that were examined, the entire melt was grown into a single crystal. If the

Jan 1, 1964

By David H. Browne

(Pittsburg Meeting, March, 1910.) NICKEL has always been a fruitful mother of problems. Previous to the year 1906 nickel was regarded as an element replacing iron in copper-mattes, and it was believed that the same laws which governed the elimination of iron could be applied-to nickel. This conception has lately undergone a complete change, and nickel in all its stages is now regarded as an element replacing copper; in other words, copper-nickel is considered now as two elements, but as one metal. When we commenced our investigations on Monel metal we made a great many experiments on the conversion of mattes, both high copper and high nickel. We studied closely the composition of the mattes and the changes produced by the blow. We found in all cases certain agreements which we believe are due to some law. Briefly stated, our conclusions are as follows 1. Nickel is not an element replacing iron in matte. 2. Nickel-copper alloys act in the matte-blow like one metal. 3. Nickel-copper alloys follow, during the matte-blow, exactly the same laws as govern. the behavior of copper alone. This brings up the question : What are the laws governing the production of metallic copper, and what are the relations copper to sulphur and iron during the Bessemer blow ?

Apr 1, 1910

By C. A. Hartnagel, D. H. Newland

The market for Pennsylvania grade showed a drop both in demand and in prices, which reacted unfavorably on New York oil production, all of which comes under that classification. The output for the year in New York amounted to 5,045,200 bbl. The production in 1937 was 5,478,000 bbl., the largest in any year for the last half century or more. Falling prices, of course, affected new drilling. They declined from $2.20 a barrel, which was posted at the start, to $1.68 in the final months of 1938. With this came a reduction in the amount of oil that would be accepted by the refineries operating in the New York fields. Conditions therefore have combined to halt, at least temporarily, the growth of oil production in the state, which had experienced a steady gain for the last 15 years or more, the yield having risen from less than 1,000,000 bbl. to the round total of 5,500,000 bbl. in 1937. Practically all the oil now obtained is from old, developed fields. No new pools have been found in the last quarter of a century or more. The larger share comes from flooding the sands. Although there are many wells that still produce without the aid of the water drive, they are small and for the most part are pumped periodically. Of late, new drilling has been restricted mainly to that required to maintain existing flood projects. Because of the high initial cost and time required to put a flood into production, the depressed condition of the market has been a serious handicap financially, and, further, has been an unfavorable influence on the planning of operations to secure the maximum recovery of the oil. Unless market conditions improve, it is certain that the effects will be shown in the yield for some time to come. Gas Developments Drilling was active in the southwestern area, chiefly in Allegany and Steuben Counties, and some notable wells were brought in that tapped the Oriskany sandstone. Altogether 42 holes were put down in the two counties, of which 31 were listed as producers and 11 were dry. The new wells gave an initial daily flow of 239,000 M cu. ft. At the close of

Jan 1, 1939

By C. A. Hartnagel, D. H. Newland

The market for Pennsylvania grade showed a drop both in demand and in prices, which reacted unfavorably on New York oil production, all of which comes under that classification. The output for the year in New York amounted to 5,045,200 bbl. The production in 1937 was 5,478,000 bbl., the largest in any year for the last half century or more. Falling prices, of course, affected new drilling. They declined from $2.20 a barrel, which was posted at the start, to $1.68 in the final months of 1938. With this came a reduction in the amount of oil that would be accepted by the refineries operating in the New York fields. Conditions therefore have combined to halt, at least temporarily, the growth of oil production in the state, which had experienced a steady gain for the last 15 years or more, the yield having risen from less than 1,000,000 bbl. to the round total of 5,500,000 bbl. in 1937. Practically all the oil now obtained is from old, developed fields. No new pools have been found in the last quarter of a century or more. The larger share comes from flooding the sands. Although there are many wells that still produce without the aid of the water drive, they are small and for the most part are pumped periodically. Of late, new drilling has been restricted mainly to that required to maintain existing flood projects. Because of the high initial cost and time required to put a flood into production, the depressed condition of the market has been a serious handicap financially, and, further, has been an unfavorable influence on the planning of operations to secure the maximum recovery of the oil. Unless market conditions improve, it is certain that the effects will be shown in the yield for some time to come. Gas Developments Drilling was active in the southwestern area, chiefly in Allegany and Steuben Counties, and some notable wells were brought in that tapped the Oriskany sandstone. Altogether 42 holes were put down in the two counties, of which 31 were listed as producers and 11 were dry. The new wells gave an initial daily flow of 239,000 M cu. ft. At the close of

Jan 1, 1939

By Stanley Lefond

Industrial Minerals, often called the Cinderella Minerals or the Building Blocks of industry continued their growth patterns through 1973, although profits were slightly lower due to the cost-price squeeze. Most of the individual reports which follow indicate growth rates of 3-15%. Surprisingly such commodities as sulfur held firm in spite of the over supply in the Canadian gas fields; cement was in short supply while the asbestos industry reported a worldwide shortage of group 4 and 5 fibers. Talc and perlite production set new records. In synopsis, 1973 was a productive year for industrial minerals. However 1974 onward appears to be one of contradiction. The unsettled conditions of world economics, the energy shortage, compounded by the Arabs oil embargo have created great problems for all industries. The high energy consuming segments of the Industrial Minerals field will be under intense pressures. On the other hand limestone, lime and perhaps trona, nahcolite might be consumed in ever increasing tonnages in SO2 removal systems connected with smelters and coal-fired power stations. The effects of the proposed changes in the staking, claiming and exploitation of federal lands by the BLM may also have serious repercussions not only to the industrial minerals field but to the entire mining industry. 1974-1975 will certainly be ear-marked as a year of frustrations and difficult decisions.

Jan 2, 1974

By Bradley Stoughton, M. Miyake

The importance of magnesium alloys as engineering materials has increased rapidly in the past few years. The most important properties of magnesium alloys are their lightness and strength, which result in their extensive use in aircraft and automobile construction. Recent progress in the metallurgy of magneaium seems to offer hope of the production of the pure metal at a reasonable cost. The use of magnesium would doubtless increase greatly if it could be produced at a cost comparable with that of aluminum. A preliminary survey of the magnesium-base alloys shows that the most promising from a practical standpoint are magnesium-aluminum and magnesium-zinc as binary alloys, and magnesium-zinc-aluminum as ternary alloys. The research reported in this paper is a preliminary study of binary magnesium-aluminum and magnesium-zinc alloys, as an introduction to a series of further investigations. Magnesium-aluminum System The magnesium-aluminum system was first studied by Boudouard,1 who merely determined the liquidus. An accepted constitutional diagram was given by Grube,2 who found a compound A13Mg4 (melting point = 462.7" C.) and two eutectics at 35 per cent. magnesium (451.6° C.) and at 68 per cent. magnesium (440" C.) Between the first eutectic and the compound a solid solution exists. This diagram was checked or supplemented by Pécheux,3 Broniewski,4 Eger,5 Schirmeister,6 Voge17

Jan 1, 1926

Report was made by the Committee of National Engineering Societies on the Reserve Corps of Engineers and it was voted that a committee of - three be formed-consisting of the President of the Institute, Dr. Henry -S. Drinker and the Secretary of the Institute-to select members in different parts of the country to-advise with the local U. S. Engineer Officers as to qualifications of applicants for the Reserve Corps of Engineers.

Jan 8, 1916