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By J. L. Bray, S. T. Ross

The paper provides electrometallurgical data on the problem of germanium removal from zinc sulphate solutions. Germanium traces have caused much concern to the zinc refiner. Confirmatory evidence of interaction between germanium and cadmium is presented. Statistical analysis of data expands its significance and enhances its value. Further research is outlined. THE literature contains many references to the effects of trace amounts of germanium in the production of electrolytic zinc. One of the authors had experience with this troublesome element as early as 1917 at Trail, B. C. In 1929, Tainton and Clayton' reported that concentrations of as little as one part per million of germanium were sufficient to cause serious losses in current efficiency. Liddell2 reported that trace amounts of germanium cause marked lowering of the hydrogen overvoltage of electrolytic zinc cells, so that commercial production was impaired. Bray3 recorded the history of germanium in relation to electrolytic zinc production, noting that concentrations below 10 ppm have been found to yield low current efficiencies and copious hydrogen evolution. Koehler' stated that germanium "when present to the extent of a small fraction of one part per million per liter, causes serious evolution of hydrogen with a corresponding reduction in current efficiency." Recently, however, S. W. Ross" reported, from Risdon, Tasmania, that "in the course of leaching . .. dissolved traces of germanium... if not removed almost completely ... increase the reversion of cadmium during the filtration of the copper-cadmium precipitate and reduce the current efficiency during subsequent analysis." The copper-cadmium precipitate referred to is the residue from the zinc-dusting purification of zinc sulphate leach solutions. In the face of such conflicting testimony and with the increasing industrial importance of pure germanium and zinc it was decided to investigate the relationship between cadmium and germanium. Furthermore, other work by the authors showed certain discrepancies to exist in the theories of Tainton, et al. In the laboratory, without marked efficiency decreases, the authors have deposited zinc successfully from solutions containing as high as 1 g per liter of germanium. This could be done only when there was no cadmium present. Preliminary investigations of the suspected rela- tionships were carried out by means of emission spectrographic analysis using a beryllium internal standard. Several solutions containing 100 g per liter of zinc, as zinc sulphate, and 1 g per liter of cadmium, as cadmium chloride, were prepared. These concentrations were on the order of those obtained during a commercial low-acid leaching process. Varying concentrations of germanium were added to these solutions so that the range of 0.0000 to 0.5000 g per liter of germanium was covered. A 250 ml sample of each solution was agitated with 2.5 g of zinc dust for 30 min, filtered, and the filtrates were examined spectroscopically. Qualitative evidences of cadmium traces were found in those filtrates which originally contained above 10 ppm of germanium. Reliability of the analytical method did not permit quantitative investigations since cad-Table I. Current Efficiencies Obtained at 0.0000 and 1.5000 G per Liter Cadmium Concentrations Ge Concentrastion,* Cd Concentration,* EtBclenoy, G per Liter G per Llter Pot 0.0000 0.0000 84.270 0.0010 0.0000 94.849 0.0050 0.0000 92.649 0.0075 0.0000 94.039 0.0100 0.0000 96.084 0.0000 1.5000 93.460 0.0010 1.5000 95.158 0.0050 1.5000 92.148 0.0075 1.5000 91.260 0.0100 1.5000 84.546 • Cd and Ge concentrations shown are those existing before zinc-dust purification. mium determination in the concentrations present in zinc-dusted solutions lacks sufficient sensitivity for reproducible results. As a consequence of the inability of the investigators to obtain acceptable results through direct quantitative analysis, an indirect approach was devised. This indirect method involved a study of the current efficiency, in a model zinc cell, as a function of the concentrations of cadmium and germanium. Variables such as cell temperature, voltage, current density, anode spacing, relative electrode area, degree of agitation, cathode preparation technique, time, acid concentration, and solution volume were held constant. Fig. 1 shows the cell used. The current was fur-

Jan 1, 1952

By F. P. Bullen

Empirical relationships between fracture stress, orientation angle, and diameter of crystal have been determined at 77°K. Orientation ranges of markedly different behavior were found—a law of constant normal stress&apos; of value a (diameter)-1/2 for the fracture of ductile crystals, and a condition of shear stress (or strain) for more brittle crystals. The observations are not consistent with current theories. An interpretation is advanced which is also applicable to observations on the effect of prestrain at room temperature on the subsequent fracture stress at 77°K and to the effect of cyclic stressing on the cleavage strength.&apos;&apos; The law of constunt normal stress&apos; and the brittle ductile transition are also explained. The interpretation is more consistent with the initiation of cracks by intersecting dislocations than with theories based on stress -concentration by dislocation arrays. ZINC single crystals are particularly suited to the study of cleavage because fracture occurs on the basal plane over a wide range of crystal orientations. Analysis of the conditions of stress and strain at fracture in crystals of different orientations should indicate which parameters control the cleavage process. Unfortunately, controversy has arisen over the correct empirical relationship between tensile fracture stress and orientation. Schmid&apos;s observations1,2 favored a &apos;law of constant normal stress&apos;, as observed in other materials.2 For zinc, however, the observed values are far below the theoretical strength and cannot represent the true limit of cohesion between neighboring atomic planes. Hence, the interpretation of such a &apos;law&apos; is not straightforward. Deruyttere and Greenough3,4 found a complex variation between tensile fracture stress and orientation; this variation did not agree with a &apos;law of constant normal stress&apos;. Two theories have been advanced to account for their observations: a) the propagation of cracks from low-angle boundaries,5 and b) the release of energy from piled-up dislocations during crack-propagation.4 The present work resolves the apparent discrepancy between the observations and shows that neither of the above theories are applicable to the tensile fracture of zinc single crystals. A phenomenological explanation, along the lines suggested by Gilman,&apos; is advanced and successfully applied to previously unexplained effects. EXPERIMENTAL DETAILS &apos;Crown Special&apos; redistilled zinc was used, except for one comparison series op tests using &apos;Tadanac&apos; electrolytic zinc. Crystals of 1 mm diam, subsequently called &apos;1 mm crystals&apos;, were grown from the melt in vacuo in precision-bore Pyrex tubes internally coated with graphite. Several specimens 1 in. long were cut from each crystal and chemically polished. Jigs were used to minimize handling strains, and crystals were mounted in the Polanyi machine the day prior to testing to allow recovery from any such strains. One-mm crystals were chemically polished for long periods to obtain 0.1 mm (approx) crystals. One-mm crystals were cemented into miniature gimbals by &apos;Araldite&apos; casting resin. The Appendix gives the reasons for using gimbals and the results obtained by other methods. More complete details of all techniques are given elsewhere.7 The symbols and terminology used are as follows: X = orientation angle (angle between tensile axis and line of greatest slope in the basal plane). T = tensile stress (on true cross-section) S,N = shear and normal stress (components of T with respect to the basal plane) ? = shear strain D = crystal diameter. The subscript &apos;f&apos; will be used to denote values at fracture. PART I-ANNEALED CRYSTALS EXPERIMENTAL OBSERVATIONS One-mm crystals were used to establish the variation of fracture stress at 77°K with orientation at fracture (Xf), Fig. 1. For 18 deg = Xf = 55 deg, a &apos;law of constant normal stress&apos; was observed. For Xf > 55 deg, the fracture condition approximated to a constant shear stress. At Xf< 18 deg, twinning occurred before fracture so that the results were not typical of homogeneous single crystals,4,8— such specimens will not be considered herein. The dependences of fracture stress upon Xf were of similar type for 6 mm,* 1 mm, and 0.1 mm crystals,

Jan 1, 1963

By A. P. Coldren, V. Biss

SINCE the r ? a transformation rates of many carbon-free ferrous alloys and low-carbon alloy steels are relatively fast, conventional equipment is not suitable for the dilatometric determination of continuous cooling transformation diagrams. On the other hand, a method based on metallographic analysis of quenched specimens would not be practicable because the various products of shear-dominated transformation are essentially indistinguishable in low-carbon iron-base alloys. Both problems may be avoided by a thermal analysis method employing gas quenching of small specimens austenitized in vacuo. The laboratory equipment employed in the present study consisted of a Tektronix Type 564 Storage Screen Oscilloscope and a Kinney high-vacuum evaporator, modified as shown in Fig. 1, to permit heating a small specimen and cooling it slowly by programmed cooling or rapidly (up to about 8000°F per sec) by a controlled quench with helium gas. The oscilloscope records the electromotive force of a 40-gage (0.003-in.-diam) Chromel-Alumel thermocouple in the specimen during cooling. The temperature at which the cooling curve begins to show the influence of the heat produced by the phase change in the specimen was arbitrarily taken as the transformation-start temperature.*

Jan 1, 1970

By David Mitchell

THE production of fluorspar is one of the smaller nonmetallic indus-tries in the United States with a capital investment-about $10,000,000. Shipments from United States mines&apos; in 1936 totaled 176,231 short tons valued at $3,111,268, an average price of $17.65 per ton. The United States produces about 40 per cent of the world&apos;s fluorspar, of which about 90 per cent comes from the Illinois and Kentucky deposits along the Ohio River.2 Further detailed information on the fluorspar industry in the United States is given by Hatmaker and Davis.28 Fluorspar is marketed according to the following relative quantities and specifications: Consump- Specifications, Per Cent Use Form tion in 1936, Per Cent CaF2 SiO2 Fe2O3 Metallurgical Gravel 79 +85 -5 or lump Ceramic,. Ground 10 +95 -3 -0,1 Acid Ground 11 +98 -1 The concentration of the coarser sizes presents relatively little diffi-culty, good recoveries being obtained with jigs and tables. However, sizes smaller than about 10 mesh cannot be successfully treated by ordinary gravity separation methods and so have been accumulating as

Jan 1, 1938

By Robert J. White

Strong&apos;s equation for calculating bottom-hole pressure reduction due to gas cutting of drilling mud is corrected, resulting in a simpler equation which is easier to use. Use of the equation is illustrated by examples. It is shown that reduction of weight of a 10 lb/gal mud by 50 per cent at the surface due to gas cutting produces only n 3 per cent decrease in hydrostatic head at the bottom of a 5,000-ft well. It is also shown that at the surface 5 volumes of air per volume of mud are required to reduce the apparent mud weight from 8.5 to 6.5 lh/gal in a 3,000-ft well. Illustrative graphs are included to show the effect of various degrees of gas cutting on apparent mud weight at depths of 2,000, .5,000 and 10,000 ft and to show variation of apparent mud weight, with depth for a 100 lb/cu ft (13.37 lb/gal) mud gas cut to 90 lb/cu ft (12.03 lb/gal) at the surface. INTRODUCTION In 1938, Strong&apos; published the following equation for calculating reduction in bottom-hole pressure due to gas cutting of drilling mud h = 1/D [p + pn/100 In p + p(1-n/100)/p(1- n-100)] where: h = depth in feet P = pressure in atmospheres at depth h due to mud column only D = hydrostatic pressure in atmospheres of a col-umn of uncut mud 1 ft high p = back pressure at well-head (in atmospheres) n/100 = fraction by volume of gas in mud at well-head at back pres-sure p This equation was recently found to contain an error due to an incor-rect expression for variation of vol-ume fraction of gas with pressure. Values calculated by the original equation are close to the correct values for small percentages of gas for which it was derived but become increasingly erroneous as the gas content increases and are completely unusable at the very high gas con-tents employed in aerated mud. DERIVATION The nomenclature used is the same as in Strong&apos;s paper. The pres-sure dP exerted by a lamina of thickness dh at a depth h ft is ex-pressed by Eq. 1 where x = volume fraction of gas at depth h dP = D (l - x)dh . . . (1) When we express x in terms of the wellhead per cent gas n, the well-head pressure p and the pressure P at depth h, the result is Eq. 2. x = (np/p+p)/(100-n) + (np/P + p) When this is substituted in Eq. 1 and rearranged to separate the var-iables the result is dh = 1/D [dp + np/100-n dp/(P + p]. Integration between appropriate lim-its results in or if the wellhead is open so that p = 1 atm and we rearrange Eq. 4, the result is loss in head = hD — P = n/100-n In (P + 1) ...(5) Eq. 5 can be solved easily by successive approximation using hD as a first approximation for P on the right-hand side and calculating a first value for loss in head. This can then be used to get a new value of P using the left-hand side of the equation. Values converge very rap-idly even for quite large values of per cent by volume gas n. EXAMPLES The effect on bottom-hole pressure of 50 per cent gas cutting of the mud in a 5,000-ft well using 10 Ib/ gal mud will be calculated, we have: h = 5,000 ft 10 X 7.48 144 X 14.7 = 0.0353 atm/ft hD = 176.5 atm n = 50 Substituting these values in Eq. 5 and using hD as a first approxima-tion of P on the right, we have, approximate loss in head = 50/50 In (176.5 + 1) = 2.30 log 177.5 = 5.17 atm. We calculate a new value of P as follows:

Jan 1, 1958

By P. D. Merica, A. N. Finn, R. G. Waltenberg

CeRtain compositions of the light, i.e., aluminum-rich, alloys of aluminum with magnesium and copper have become quite well known within the past ten years under the name of duralumin. These alloys are used for rolling and forging and can be so treated as to develop quite remarkable mechanical properties. Thus a properly heat-treated alloy containing about 4 per cent. of copper and about 0.5 per cent. of magnesium, rolled into sheet or rod, will have a tensile strength of approximately 55,000 1b. per sq. in. (3866 kg. per sq. cm.) with an elongation in 2 in. (50.8 mm.) of about 15 per cent. This alloy, duralumin, was developed by Wilm,1 and its properties more fully described by Cohn.2, The authors considered it worth while to investigate the mechanical possibilities of the light alloys of two somewhat analogous ternary series; namely, of aluminum-magnesium-nickel and aluminum-magnesium-manganese, to study the effect of variation of composition upon mechanical properties within the alumimum-rich group of the aluminum-magne-

Jan 1, 1921

By Edward H. Robie

In late November and early December a considerable portion of our time was devoted to obtaining a business manager for Institute headquarters. The advisability of creating such a position was suggested in 1949 in the report of the Johnson committee. In that year, however, the Institute had a deficit of $72,000 so every effort was made to minimize expense. At that time most of the duties that normally would be assumed by a business manager were given to Newell Appleton who became office manager, convention manager, purchasing agent, and assistant to the secretary. So many responsibilities were his that he could not devote the necessary time to all of the many things that needed attention. H. H. Vasoll, representing a firm that made a study of Institute head office procedures early last fall, made a recommendation that "a business manager and controller from outside the present organization" be obtained, who would supervise the work of accounting, addressograph, purchasing, book and journal orders, filing, and mailing depts. He further recommended that Mr. Appleton be made administrative secretary, in which position he would act as head of an "Institute Activities Dept." He would devote his time to convention planning, meeting arrangements, travel accommodations, membership control and promotion, and public relations, and would assist the Secretary on special problems. Thus, Mr. Appleton retains some of his former responsibilities and will take more of the load off our shoulders in the conduct of affairs at Institute headquarters. The rest of his former work will be in the province of the newly created "Business Office Dept." Peter J. Apol is the man finally selected for the post of business manager. He is a young man of 32, a native Michigander and a graduate of the University of Michigan where he received a B.S. degree in business administration in 1940. He then spent three years in the Navy and has the rank of Lieutenant in the U. S. Naval Reserve. Three more years were spent in the U. S. Maritime Service as chief purser, and another year as chief paymaster for the Pope & Talbot Steamship Co. The past four years have been spent as head of the Greenland Construction Co., Greenland, N. H., chiefly engaged in building construction. Mr. Apol will endeavor to increase the efficiency of Institute headquarters operations and remove all possible causes for complaints of individual members. He will coordinate as seems advisable the work of various departments and install such modern business office machinery as seems applicable to our needs.

Jan 1, 1952

By M. T. Hepworth, W. B. Sample

HYDROGEN solubility and linear contraction measurements were made at constant temperature on an alloy of titanium of constant oxygen-to-titanium molal ratio but variable hydrogen content. A cylindrical specimen of titanium (0.25 by 1.6 in.) containing 0.75 at. pct 0 and less than 0.03 at. pct N was cast from a master button of iodide process titanium which had been alloyed with titanium dioxide. Four vacuum fusion analyses, which were made along the length of the cylinder after the hydrogen solubility studies were made, revealed a variation of oxygen content of less than 0.02 at. pct. The specimen was introduced into a quartz furnace tube, annealed and outgassedat 1050"~ for about 1 hr, and then held at 800" * 0.5" for about 30 hr, during which latter time experimental data were taken. The leak rate to the furnace chamber was not sufficient to contaminate the specimen during the run as determined by leak-rate studies and vacuum fusion analyses for oxygen and nitrogen before and after the runs. The furnace chamber was attached to a modified Sieverts apparatus used to introduce measured quantities of purified hydrogen to the specimen. A quartz pushrod transmitted changes in length of the specimen to a Chevenard dilatometer. The push-rod passed through a vacuum grease seal to the dilatometer which amplified motion of the rod by a factor of 319. During hydrogen addition, the pushrod did not contact the specimen. Measured quantities of hydrogen were added to the specimen and equilibrium hydrogen pressures recorded as a function of hydrogen content. The solubility data, which appear in Fig. 1, agree well with a separate investigation made with a different apparatus. The solubility limit of the hcp a phase appears as an abrupt discontinuity in slope at 3.4 at. pct H. The solubility plot has been extended as a dashed line at this discontinuity in order to emphasize the discontinuity. The hydrogen content at which bcc P appears is not clearly defined. An arrow indicates solubility data were taken upon hydrogen addition. Upon reaching the arbitrary maximum hydrogen content of the run, the quartz pushrod was pressed against the specimen in order to record the change in length with hydrogen removal. A pressure of about 100 g per sq cm was required to overcome the friction of the vacuum seal in order to obtain reproducible linear contraction data. The contraction ratio ~2/1", change in length divided by original length, was set equal to zero for the maximum hydrogen content. The relative contraction of the specimen was observed upon removal of hydrogen in the following manner. The system was opened to the pumps for a few seconds and an unknown quantity of hydrogen was removed. The system was then isolated from the pumps by closing a stopcock and allowed to return to equilibrium. When the temperature returned to 800°C, the pressure stabilized, and contraction ceased, measurements of contraction and pressure were made. The hydrogen content of the specimen was then deduced by measuring the equilibrium PIydrogen pressure and referring to the solubility plot. Linear contraction was then plotted against interpolated values of atomic percent hydrogen. The justification for this procedure is the established reversibility of the hydrogen equilibrium.&apos; Uniaxial compression was assumed to have no effect on hydrogen pressure. The isothermal linear contraction data are plotted on Fig. 1. An arrow indicates data were taken upon removal of hydrogen. The solubility limits of the two phase a i /3 region can be identified by discontinuities ill slope of the dilatometric plot at 9.1 and 3.4 at. pct H, agreeing well with other studies.&apos; Dashed extensions of the plots emphasize the discontinuities. Isothermal studies of expansion made upon hydrogen addition gave curves of much smaller slope and less pronounced discontinuities. A uniaxial compressive stress tends to accentuate volume changes in going from the more open bcc phase to the hcp phase.2 Incomplete data on ex-

Jan 1, 1962

Discussion of the paper of Blarney Stevens, presented at the Butte meeting, August, 1913, and printed in Bulletin No. 79, July, 1913, pp. 1285 to 1303. F. L. GRAMMER,Leesburg, Va. (communication to the Secretary*):¬ Mr. Stevens refers to an explanation of parallel jointing by W. 0. Crosby, which I noted when reading one of his excellent text books. It seemed to me earthquakes were not a satisfactory explanation, and I looked up several authorities; but I never realized how small the usual amplitudes were until Mr. Stevens presented his paper. Several letters to the U. S. Geodetic Survey showed me there were very few records of tidal movements of earth crust in the United States. Altitude and latitude would be influencing factors; but this diurnal movement must exceed earthquake amplitudes, besides being more nearly universal. My inquiries brought the answer that the major directions of jointing had not been extensively tabulated. If major directions of jointing were recorded-with notes as to angle with mountain chain, or North Star, and distance between joints, with nature of rock and maximum and minimum tidal up-heaval-some interesting relations might be made manifest.

Jan 11, 1913

By E. F. Ketterer, D. B. Collyer, A. B. Wilder

The microstructural stability of 59 carbon and low alloy steels after 34,000 hr exposure at 900&apos; and 1050°F, including the weld heat-affected zone, is discussed. The tensile and creep rupture properties of the parent metal of many of the steels before and after 10,000 hr exposure are presented. SEAMLESS pipe has been used for many years at elevated temperatures. When seamless first began to be used, operating temperatures and pressures were relatively low and the steel produced adequately met the existing requirements. The need for knowledge of creep properties and graphitiza-tion was nonexistent. Today the requirements for tubular products have changed considerably. Operating temperatures and pressures are increasing continually and corrosion, particularly at high temperatures, presents a problem. Carbon steels have, under these conditions, certain economic advantages particularly in oil refinery use. However, the use of low alloy steels in the generation of steam power has increased appreciably due to the influence of molybdenum on creep strength and the control of graphitization with chromium. The behavior of carbon and certain low alloy steels after long periods of exposure at 900° and 1050°F (480° and 565°C) has been investigated. The steels were examined before and after 10,000 to 34,000 hr exposure. Results obtained with material exposed at 1200°F (650°C) are not presented due to the severe oxidation and resulting decarburiza-tion after long periods of exposure. The graphitization characteristics of carbon and low alloy steels are of fundamental concern to the users of these materials. This is particularly true where welded joints are employed. In order to evaluate properly the behavior of steels at elevated temperatures, it is desirable to employ not only long periods of exposure under controlled conditions, but to use material with known properties and steelmaking practices. The purpose of this investigation has been to study the microstructure of the weld and the tensile and creep rupture properties of the parent metal after long periods of exposure at elevated temperatures. In the report&apos;.&apos; of a previous investigation data were presented on the microstructure, impact strength, hardness, and oxidation characteristics after 10,000 hr exposure at elevated temperatures. When this investigation was planned, methods for controlling the graphitization characteristics of steel were not established and, therefore, a number of special alloy steels were included in the study. During the exposure of these steels, the influence of aluminum in accelerating the rate of graphitization and the inhibiting power of chromium were established by various investigators. Also, the vanadium-bearing steels, because of their outstanding creep properties, received attention. As a result of these developments, considerable progress has been made in the field of high temperature tubular products, and the necessity for special alloys to prevent graph-itization has been restricted largely to the use of chromium. Material Chemical analysis, deoxidation treatment, and austenitic grain size of the 59 steels discussed in this paper are shown in Table I. The steels were forged to 1x1 in. bars with the exception of steels 12B, 12DX, 12DY, 12DZ, 70, 70A, 72 to 78, 82, and 83 which were machined from heavy wall pipe. All bars were surface ground before exposure. Heat treatment before exposure is shown in Table 11. The majority of the steels included were melted in either a basic open hearth or basic electric furnace; how-

Jan 1, 1955

By Arthur C. Spencer

IN extension of a suggestion already made to account for certain features observed in the Juneau gold-belt in southeastern Alaska,&apos; it is the object of the present paper to indicate in detail certain conditions in which deformation of rocks under their own weight might lead to the production of fractures in which veins could be deposited. A direct, uniformly-distributed pressure of sufficient intensity applied to an elastic brittle mass offering strong resistance to deformation produces rupture. In a material of ideal properties the surfaces of rupture under such pressure would be shearing planes inclined at 45° to the line of force, unless there be preliminary deformation, in which case this angle would be greater than 45°. This general conclusion, resting upon ana¬lytical mechanics, is completely supported by the results obtained by Daubrée in experiments upon the deformation of wax and resin prisms under compression. Let us then first con¬sider one of Daubrée&apos;s diagrams. In the case illustrated in Fig. 1, four sets of fractures in two appproximately right-angled pairs (that is to say, in conjugate sets) were produced by end-wise compression of the square cross-sectioned prisms. These fractures cut the axis of compression at approximately equal angles, not varying greatly from 45°. The location of the four sets of fractures is obviously determined by the shape of the prism, since the material in each corner acts in a way as a buttress, permitting the bulging to take place most readily on the sides. By limiting the directions in which bulging may take place, results of a more simple nature could be obtained. Take, for instance, a square prism and place it between two fixed and

Nov 1, 1905

By F. R. Hensel

THE absorption of oxygen by molten metals is a quick and convincing method to determine the metallurgical characteristics of various types of furnaces.1 The investigation was restricted to the use of coreless induction furnaces. A major variable in induction furnace practice is the frequency and its influence was studied by comparing melts made in a 5000-cycle and a 60-cycle induction furnace respectively.2 The authors are not aware that such a comparative study has been made before and therefore present this paper in the belief that the results will be of general interest. ANALYTICAL METHODS FOR DETERMINATION OF OXYGEN IN NICKEL An analytical procedure for determining NiO by a quick and simple, laboratory method has been worked out in collaboration with Dr. Herty, of the Pittsburgh Station of the Bureau of Mines. It was found that Dr. Herty&apos;s aluminum method as used for the. determination of FeO in iron and steel was very suitable for use with nickel if instead of hydrochloric acid a 10 per cent solution of nitric acid is used for bringing the metal into solution. Essentially this method involves deoxidizing the nickel-oxygen alloy with aluminum (2Al + 3NiO = Al203 + 3Ni) and determining the resulting Al203 by a residue analysis. The original oxygen content can then be calculated from the amount of Al-20,. The method as suggested by Dr. Herty3 is referred to in the present paper as method B. A slight modification of method Bled to the application of method A, a description of which is given below according to F. W. Beiter?:3

Jan 1, 1932

By John L. Schroder

In selecting the best system of mining for a particular operation, many different factors must be considered. The system to be finally selected should be that which provides: 1) The highest possible degree of safety for mine personnel. 2) The lowest cost per ton of product. 3) The maximum coal production per man-shift. 4) The most suitable quality of final product, considering its intended use. 5) The maximum percent recovery of coal per acre of reserve consistent with cost and subsidence rights. 6) Consideration for the ecology of the area. Some of the important factors to be considered when choosing a method of mining are: 1) Amount of cover over the coal seam. 2) Type of the rock in the overburden. 3) Characteristics of the coal seam including: (a) the thickness of the coal seam; (b) the nature and location of any impurities or irregularities; (e) the dip (or pitch) of the coal seam; (d) the nature and direction of any definite cleavage ill the czoa1 seam; (e) the hardness of the coal; (f) the structural strength of the coal; and (g) the presence, anti amount, of explosive gas (methane). 4) Quantity of water likely to be encountered in the mining operation. 5) Nature and strength of the roof (top) over the coal seam. 6) Nature and strength of the floor (bottom) under the coal seam. 7) Any previous or concurrent mining in seams above or below the coal seam to be worked. Information on items 1-7 may be obtained in several ways. Topographical and geological reports and maps of the area are generally available

Jan 1, 1973

By H. M. Morse

Mississippi, during the year 1941, experienced the greatest diversity of oil activity since the beginning of oil interest in the state—core tests for exploration, core tests for sulphur, continued drilling at Tinsley for production, and wildcatting, which brought to light two new oil fields and two new salt domes. There were 45 wildcat wells drilled in 1941, which showed greater results and findings geologically than the 85 drilled in 1940. Tinsley Oil Field (Yazoo County).—The Tinsley oil field, with its boundaries fairly well defined now, is 8 miles long and 3 miles wide at its widest point. During the past year 213 producing wells were completed, which brought the total number of producers in the field by the end of 1941 to 325 wells. Seven producing sands have been logged, with a total average thickness of 30 ft. of oil sand. The producing formations are the Selma, Eutaw and Tuscaloosa. The average total depth of the wells is 5012 ft. The average gravity of the oil is 35.4°. Production for 1941 was approximately 15,500,000 bbl. of oil. Vaughan-Pickens Oil Field (Yazoo County).—At the end of 1941 only three wells were Producing in this field, the fourth having been abandoned. The total production for the field for the year was approximately 250,000 bbl. of oil. The producing sand is the Wilburn, in the Eutaw formation. Cary Field (Sharkey County).—The British American Oil Producing Co. completed, on Sept. I, 1941, its F. B. Houston No. A-I well, sec. 23, T. 11 N., R. 7 W. It is

Jan 1, 1942

By H. M. Morse

Mississippi, during the year 1941, experienced the greatest diversity of oil activity since the beginning of oil interest in the state—core tests for exploration, core tests for sulphur, continued drilling at Tinsley for production, and wildcatting, which brought to light two new oil fields and two new salt domes. There were 45 wildcat wells drilled in 1941, which showed greater results and findings geologically than the 85 drilled in 1940. Tinsley Oil Field (Yazoo County).—The Tinsley oil field, with its boundaries fairly well defined now, is 8 miles long and 3 miles wide at its widest point. During the past year 213 producing wells were completed, which brought the total number of producers in the field by the end of 1941 to 325 wells. Seven producing sands have been logged, with a total average thickness of 30 ft. of oil sand. The producing formations are the Selma, Eutaw and Tuscaloosa. The average total depth of the wells is 5012 ft. The average gravity of the oil is 35.4°. Production for 1941 was approximately 15,500,000 bbl. of oil. Vaughan-Pickens Oil Field (Yazoo County).—At the end of 1941 only three wells were Producing in this field, the fourth having been abandoned. The total production for the field for the year was approximately 250,000 bbl. of oil. The producing sand is the Wilburn, in the Eutaw formation. Cary Field (Sharkey County).—The British American Oil Producing Co. completed, on Sept. I, 1941, its F. B. Houston No. A-I well, sec. 23, T. 11 N., R. 7 W. It is

Jan 1, 1942

By D. Moskowitz

IN the course of a general investigation of boride systems, sponsored by the Office of Naval Research, various vanadium boride powders of relatively good purity were prepared which could be used for a determination of the phases present. The X-ray pattern of one of these lots showed, in addition to the known VB1 and VB22 phases, an additional phase, almost certainly of composition V3B4, isomorphous with Cr3B4, Cb3B4, Ta3B4, and Mn3B,. Its pattern fitted in well with the indices worked out by Kiessling for Mr3B4.3 The unit cell for this new compound is orthorhombic, with the dimensions a = 3.030A, b = 13.18A, c = 2.986A7 V=119.2A.&apos; Table I lists the X-ray diffraction data for V.3,.

Jan 1, 1957

By L. L. Wyman

Since the presentation, by the writer, of the initial paper on the embrittlement of copper,1 the subject has been investigated further along two separate lines. The first series of investigations involves the "double-deoxidized" coppers, while the second series is devoted to single deoxidizers other than those used in the investigations reported upon last year. The object of these experiments is to develop a type of copper that will show the minimum of detrimental effects after having been exposed to alternate oxidation and reduction. The fabrication of this material necessitates the use of alternate oxidizing and reducing atmospheres, at temperatures ranging up to 900" C. Following this treatment it is essential that the soundness and strength of the copper be unimpaired, even in sections of only a few thousandths of an inch in thickness. Materials The ensuing report embodies three separate groups of materials, which may be classified as follows: 1. Double-deoxidized copper using silicon and calcium boride. 2. Copper deoxidized with calcium. 3. Double-deoxidized copper using constant calcium content (0.075 per cent) plus silicon, or calcium boride. Last year, T. S. Fuller, of the General Electric Research Laboratory, suggested that if a properly deoxidized copper had sufficient deoxidizer residual in the material, this excess material might increase the resistance of the copper to the oxidation reduction cycle. In consequence of this suggestion, two small lots of "double-deoxidized" copper were prepared. The first, lot A, was made by adding 0.03 per cent silicon as the deoxidizer, following this by an addition of 0.55 per cent calcium boride immediately before pouring. The second, lot B, contained the same ingredients, but these were added in the reverse manner. Inasmuch as these lots were tested separately from the materials about to be described, it must be borne in mind that the materials cannot be grouped together, and are not directly comparable.

Jan 1, 1933

By Harry Seltz

SEVERAL investigators have measured the heat capacity of cementite, using different methods of attack, but the agreement between the values obtained cannot be considered good. Naeser1 has made measurements of "average heat capacities" of iron carbide between 1026° and 85° K., using a water calorimeter. His computed true specific heat at 78.1° K. is 11.22 cal. per gram-formula mass, which, if correct, is much too high for any reasonably accurate extrapolation to 0° K. The cementite used by Naeser was obtained from a steel containing 0.9 per cent carbon, by electrolytically dissolving out the iron in a neutral bath of ferrous chloride. The cementite remained as a coarse, crystalline, gray powder. Andes" has measured the specific heat of iron carbide, from 102° to 323° K., as it exists in steel. The specific heats of several slugs of steel of known iron carbide content were determined, and the specific heat of the iron carbide (Fe3C) calculated by plotting specific heat versus percentage of carbon, and extrapolating to pure Fe3C (6.7 per cent C). The heat-capacity values for temperatures below 100° K. were obtained by comparing the temperature-specific heat curve for Fe3C to that of Fe. Since the two were very similar in the range examined experimentally and approach more closely at low temperatures, it was assumed that near the absolute zero the form of the curve for Fe3C would be similar to that of Fe. Andes calculates for the entropy of Fe3C, S298 = 23.55 e.u. The heat of formation of Fe3C has been studied by several workers. Kelley&apos; has reviewed these measurements and calculations, and selects those of Roth4 and Naeser5 as worthy of most consideration. Roth has given ?H = 5400 cal. ± 30 per cent as a result of his own and other work. Naeser has determined the heat of formation from Fe and different forms of carbon, and for graphite (ß) he finds OH = 5600 cal. Kelley accepts the rounded figure ?H = 5500 as the heat of formation at 298.1° K., but this value is quite uncertain.

Jan 1, 1939

By S. D. Michaelson, Eric Sinkinson

Many of the magnesite ores of the western part of the United States contain such large amounts of silica and hydrous silicate minerals that the value of the ores is either low or nominal. Expensive and carefully controlled mining methods are necessary to prevent excessive dilution of the higher grade ores by introduction in mining of small pieces of the hanging walls or footwalls of the deposit. This difficulty is further complicated by the various states of decomposition of the country rock of the deposits in which many of the ores occur. The problem the authors attempted to solve arose from a request to float an impure magnesite containing varying proportions of siliceous gangue with calcium carbonate. The ore is normally enclosed in serpentine masses, somewhat decomposed, and in mining it wall rock is incidentally added, so that variable amounts of siliceous material occur in the samples. The silica, alumina, and iron oxide are so closely associated with the magnesium carbonate in the magnesite that ordinary mechanical separation at coarse mesh sizes is of no avail. It is well known that calcium carbonate can be floated by suitable reagents, therefore it seemed reasonable to suppose that magnesium carbonate minerals would behave in a similar manner, but experimental trial proved that this supposition was unfounded. Therefore the first step in the problem was to find out what differences of behavior there were between magnesium and calcium carbonates under flotation conditions, or when suspended in water. In water at 18" C. magnesium carbonate is slightly more soluble than calcium carbonate; in fact, MgCO3 is soluble to the extent of 0.0106 grams in 100 c.c. of water at 18" C. and CaCO3 to the extent of 0.0013 grams. However, magnesium carbonate in water gradually changes to the basic carbonates of a composition (3MgCO3.Mg(OH)23H2O) or (4MgCO3.Mg(OH)25H2O), depending upon conditions, and calcium carbonate to calcium hydroxide, Ca(OH)2. The relative solubilities of these hydroxides in water are the reverse of the solubilities of magnesium and calcium carbonates. The range in published figures for solubility

Jan 1, 1938

By S. D. Michaelson, Eric Sinkinson

Many of the magnesite ores of the western part of the United States contain such large amounts of silica and hydrous silicate minerals that the value of the ores is either low or nominal. Expensive and carefully controlled mining methods are necessary to prevent excessive dilution of the higher grade ores by introduction in mining of small pieces of the hanging walls or footwalls of the deposit. This difficulty is further complicated by the various states of decomposition of the country rock of the deposits in which many of the ores occur. The problem the authors attempted to solve arose from a request to float an impure magnesite containing varying proportions of siliceous gangue with calcium carbonate. The ore is normally enclosed in serpentine masses, somewhat decomposed, and in mining it wall rock is incidentally added, so that variable amounts of siliceous material occur in the samples. The silica, alumina, and iron oxide are so closely associated with the magnesium carbonate in the magnesite that ordinary mechanical separation at coarse mesh sizes is of no avail. It is well known that calcium carbonate can be floated by suitable reagents, therefore it seemed reasonable to suppose that magnesium carbonate minerals would behave in a similar manner, but experimental trial proved that this supposition was unfounded. Therefore the first step in the problem was to find out what differences of behavior there were between magnesium and calcium carbonates under flotation conditions, or when suspended in water. In water at 18" C. magnesium carbonate is slightly more soluble than calcium carbonate; in fact, MgCO3 is soluble to the extent of 0.0106 grams in 100 c.c. of water at 18" C. and CaCO3 to the extent of 0.0013 grams. However, magnesium carbonate in water gradually changes to the basic carbonates of a composition (3MgCO3.Mg(OH)23H2O) or (4MgCO3.Mg(OH)25H2O), depending upon conditions, and calcium carbonate to calcium hydroxide, Ca(OH)2. The relative solubilities of these hydroxides in water are the reverse of the solubilities of magnesium and calcium carbonates. The range in published figures for solubility

Jan 1, 1938