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The State Mining Experiment Station, Missouri School of Mines and Metallurgy, Rolla, Mo Charles H. Fulton, Director of the School of Mines Martin H. Thornberry, Director of the Mining Experiment Station. From the State Mining Experiment Station are issued all the general and technical bulletins of the School of Mines The latest bulletin containing a complete list of publications will be sent upon application to the Director of the Station Residents of the state may obtain bulletins as issued without charge, or may ask to be placed on the mailing list. Nonresidents should write to the Director for further information concerning specific bulletins. From the long list of bulletins the following have been care¬fully selected as being most likely to interest the geologist and the mining engineer. Vol 8, No. 1 (1916), Bibliography of concentrating ores by flotation, by J Cunningham, vol 1, No 3 (1912), Some apparatus and methods for demonstrating rock drilling and the loading of drill holes in tunneling, by L E Young, vol 2, No 1 (1915), Comparative tests of piston drill bits, by C R Forbes and L M Cummings; vol 2, No 3 (1916), Cupellation losses in assaying, by H. T Mann and C. Y Clayton; vol 4, No 1 (1917), The hydrometallurgy and electrolytic precipitation of zinc, by F D. James; vol 4, No 2 (1917), The effect of additional agents in flotation, pt 1, by M. H. Thornberry and H T. Mann, vol 5, No 1 (1919), The carbonization of Missouri cannel coals, by H L. Dunlap, K. K. Kershner and V. X Smiley. Vol 5, No. 4 (1921), Coal mining methods in Missouri, by W W Weigel, vol 6, No 1 (1921), The problem of the St Peter sand¬stone, by C L Dake, 50 cents, vol 6, No. 2 (1922), Bibliography on the electrothermic metallurgy of zinc, by B M. O'Harra, vol 6, No. 4 (1923), Experiments on the distillation of zinc from complex zinc-lead-silver ores, by B M. O'Harra and E S. Wheeler, vol 7, No 3 (1924), Underground loading devices, by C. E. van Barneveld, 81; vol 7, No. 4 (1924), Briquetting of zinc ores, by B. M. O'Harra; vol. 8, No 2 (1925), A treatise of Missouri clays, by M. H. Thornberry.

Jan 1, 1933

By M. E. Straumanis, J. -P. Krumme

In basic ([KOH + KCl] with a total polarity of 2) or acidic (2N H2SO4) electrolytes and at anodic current densities of more thun 2 to 4 ma per sq cnz, n-type GaAs single crystals of lozo resistivity preferentially dissol~je forming etch tunnels with triangular or civc~ilay cross sections and of a width between 0.5 arid 5 p. These etch tunnels are oriented along any one of the four possible (111) directions of GaAs. However, their growth occurs only in one direction of a given (111) whick apparently is determined by the atomic sequence Ga —As (and not the rezlerse) in respect to an individual valence bridge in the crystal. It is concluded from comparison with the cubic lattice structure of GaAs that the etch tunnels represent macroscopic evidence for the tetrahedral bonds and their polar properties. If the anodic current density is increased the tunnel fomation results in the development of a fibrous surface layer consisting of GaAs. The latter separates frorn the substrate (in an anodic s~irface disintegration process) by the growth pressure of an As,0, filnz forming in the interior of the fibrous layer, 100 to 200 µ under the surface, at more than about 50 ma per sq cni. The fibrous GaAs film has the same crystallographic orientation as the substvate and represents a skeleton of the original crystal. Since the etch-tunnel density in a separated GaAs layer is about 108 c?n-', and the etch tunnels develop only along (111) in a given polar direction, it is assurraed tlmt the dislocations have no influence on the growth of these tunnels. ElECTROLYTIC treatment of smooth surfaces of poly- and single-crystalline GaAs at high anodic current densities causes the formation of porous surface layers.' This phenomenon suggests comparison with effects being observed with magnesium,' indium,, gallium,4 and aluminum5 and known as "anodic disintegration". The purpose of the present paper is to explore and to explain the reasons for the formation of such surface layers on GaAs and, in particular, to investigate the influence of the lattice polarity of this III-V compound semiconductor in the (111) direction on the anodic dissolution behavior. GaAs SINGLE CRYSTALS For the experiments described below GaAs single crystals from the Monsanto Co., St. Louis, Mo., were used. Their impurity levels were below 1 ppm and their dopant levels between 1 and 100 ppm. They were grown in (111) using the Czochralski or the gradient-freeze technique. The crystals had n-type conductivity and electric resistivities between 1 and 5 ohm-cm. EXPERIMENTAL The GaAs single-crystal rods were cut perpendicularly to (111) into wafers of about 1 mm thickness using a wire-blade crystal slicer and an aqueous slurry of Sic or a diamond saw. The orientation of the faces of these wafers were checked by Laue back-reflection patterns. If there was a deviation from (111) the faces were abraded under a certain angle using grinding paper and distilled water. The damaged surface layer was removed from each crystal by chemical etching with a mixture of 1HF:1HNO3: 1H20 or 2HF:1HNO3:2HAc (glacial). {110) faces were obtained by mechanical cleavage, producing surfaces which did not require a further treatment. The GaAs wafers were mounted using "alligator" clamps instead of soldered electrical contacts.' Only the bare crystal surfaces were dipped into the electrolyte. The clamps were coated with insulating wax to prevent any contact with the electrolyte. The experiments were carried out in aqueous 2 N H2so4,' or in an aqueous solution of KOH and KCl1 (1 mole KOH + 1 mole KCl in 1000 cu cm solution). Anodic current densities up to several hundred ma per sq cm were applied for periods between 30 sec and 2 hr. For the purpose of investigating the initial steps of disintegration the anodic current density applied never exceeded 20 ma per sq cm. The films which partially separated from the anodic surfaces under high-field conditions were treated with KOH to further their detachment by dissolving the As2O3 formed. The washed and dried films were pasted to strips of filter paper, and Laue pictures were made. The back-reflection patterns obtained were compared with those of the original anode surface before and after anodic dissolution. Furthermore, space reciprocal lattices7 were constructed from asymmetric rotation crystal patternsa which permitted the determination of the crystallographic orientation of the detached films of the corrugated anodic surfaces. The disintegration products were identified from assymmetric powder patterns.8 The polarity of the {111) faces was determined by chemical etching with mixtures of 1HF:1H2O2(30 pct): 2H2O or 1HNO3:2H2O. Different patterns on each of two inverse (111) sides appeared.'-l8 The correlation of these patterns to the Ga{111) or the As(111) side has already been established by the use of light figures,18-20 by X-ray diffraction near the absorption edges of gallium and arsenic,'lmZ4 and by LEED measurements.25 The geometric structure of these surfaces and the interior of the anodically attacked crystals were observed and photographed with a high-power microscope using oil immersion objectives up to magnification of X1720.

Jan 1, 1968

By A. Boltax

The effect of cold work on the electrical and magnetic properties of solution-treated and aged Cu-Fe alloys was studied. The electrical resistivity of solution-treated and of aged Cu-1.7 wt pct Fe samples increased by up to 25 and 140 pct, respectively, follozcing a 55 pct reduction of area. The principle contributions to the increase of resistivity of the solution-treated and aged samfiles are examined. Measurements of the .saturation induction, coercive force, and stacking fault Probability are also reported. 1 HIS paper is the second in a series which examine the behavior of the electrical and magnetic prop- erties of Cu-Fe alloys. The first paper1 was primarily concerned with the effects of thermal treatment whereas the present paper examines the effects of cold work on solution-treated and aged Cu-Fe alloys. The effects of cold work on the transformation of the coherent fcc iron precipitate to the ferromagnetic form2 and the coercive force and remanence3 have already been described, but the unusually large increases in resistivity (up to 220 pct) which occlir with cold work have not been reported previously. EXPERIMENTAL METHOD The methods used for alloy preparation, heat treatment, and electrical and magnetic measurements are described elsewhere.1 The specimens, initially 4-in. lengths of 0.0625-in. diam wire, were cold worked by swaging in hardened steel dies. Following each reduction, the samples were etched lightly in hydrochloric acid to remove surface con-

Jan 1, 1962

By John T. Galey

In southwestern Pennsylvania 151 wells1 were completed during 1938, a total of 61 less than the preceding year. Of this number 81 were gas wells and 28 oil wells, which shows a considerable decline from 1937, when 108 gas wells and 64 oil wells were completed. However, 42 dry holes were drilled during 1938, which is two more than the previous year. Shallow Development—Gas No new extensions to old pools, or new wells that would indicate any substantial reserves, mere found during the year. However, a number of commercial wells and many dry holes were drilled to the Big Injun sand in Menallen township, Fayette County. One well had an initial open flow of 6 million cu. ft. In Rich Hill township, Greene County, one well producing, from the Big Injun sand, 2 million cu. ft. was brought in. Several other gas wells were completed in Shaler township, Alleghany County and Center township, Greene County, both of which had initial open flows of 1 million cu. ft. from the 30-ft. sand. Another well, in Aleppo township, Greene County, had an equal volume from the Gordon Stray sand. Oil Development has proceeded at a retarded rate because of the low price of Pennsylvania-grade crude. A total initial of only 205 bbl., an average of 7.3 bbl. per well, was developed. This is 1785 bbl. less than during 1937 and no new repressuring operations have been contemplated to prevent the declining production. The average price received for oil was $1.56 per barrel, with a high of $1.88 and a low of $1.34. This oil costs $1.94 per barrel2 to produce. The average price paid for Bradford

Jan 1, 1939

By John T. Galey

In southwestern Pennsylvania 151 wells1 were completed during 1938, a total of 61 less than the preceding year. Of this number 81 were gas wells and 28 oil wells, which shows a considerable decline from 1937, when 108 gas wells and 64 oil wells were completed. However, 42 dry holes were drilled during 1938, which is two more than the previous year. Shallow Development—Gas No new extensions to old pools, or new wells that would indicate any substantial reserves, mere found during the year. However, a number of commercial wells and many dry holes were drilled to the Big Injun sand in Menallen township, Fayette County. One well had an initial open flow of 6 million cu. ft. In Rich Hill township, Greene County, one well producing, from the Big Injun sand, 2 million cu. ft. was brought in. Several other gas wells were completed in Shaler township, Alleghany County and Center township, Greene County, both of which had initial open flows of 1 million cu. ft. from the 30-ft. sand. Another well, in Aleppo township, Greene County, had an equal volume from the Gordon Stray sand. Oil Development has proceeded at a retarded rate because of the low price of Pennsylvania-grade crude. A total initial of only 205 bbl., an average of 7.3 bbl. per well, was developed. This is 1785 bbl. less than during 1937 and no new repressuring operations have been contemplated to prevent the declining production. The average price received for oil was $1.56 per barrel, with a high of $1.88 and a low of $1.34. This oil costs $1.94 per barrel2 to produce. The average price paid for Bradford

Jan 1, 1939

By R. W. Brauchli

The author has made a statistical analysis of the relations between recovery and length of cores, diameters of cores and of drill pipe, and cost of coring under different contractual conditions. The data are presented in tabular form. The length of the core appears to play a minor part in the percentage recovered, with a tendency to lower percentages with increased core length; approximately 50 per cent of the length cored is normally recovered if the cores are more than 2 in. in diameter. The diarneter of the core has a more pronounced influence on the recovery; 1 3/8-in. cores average 29.1 per cent, 2 1/8 -in. core 53.4 per cent and 3 1/8-in. cores with 6 5/8-in. drill pipe 68.5 per cent. Where 31/8-in cores were taken with smaller diameter drill pipe, i. e., 4 1/2 - in. drill pipe in 8 1/4-in. hole, the recovery dropped to 49.8 per cent, indicating that the more rigid drill pipe favors good core recovery, a conclusion also borne out by the results obtained in using large drill pipe for smaller diame-ter cores. Surprisingly good recoveries were obtained from both the Johnson and Simpson sands; shale, limestone and dolomite each gave less then average recoveries. No serious fishing jobs resulted from coring operations. Attention is called to the need of a core drill which will make it possible to drill a full-sized hole while coring, and thus reduce the cost of cores. Data pertaining to core drilling should be consistently recorded, such as, diameter of drill pipe and collar, diameter of core, recovery, size of cutter heads, type of core-barrel, coring time, speeds of rotation and of pumps, weight on core-barrel, etc.

Jan 1, 1933

By M. F. Trice

PYROPHYLLITE is a hydrous aluminum silicate (A12Si4O10(OH)2)1 that occurs in both the foliated and the massive forms. The foliated variety resembles talc in that it has a greasy feel, a pearly luster, perfect basal cleavage, and usually is white, although in some deposits apple green, gray, brown, russet, and nearly black specimens may be found. The massive deposits of pyrophyllite yield pearl gray to light tan aggregates, some of which are so friable that they may be crushed with the hands into a fine gritty powder. Frequently specimens of the massive variety are studded with crystals of radial structure. The mineral has a specific gravity of about 2.7 and a hardness of 1 on Mohs' scale.1 The chemical composition of commercial pyrophyllite reflects the mineralogy of the deposits, which, according to Stuckey,2 contain pyrophyllite and quartz, together with chloritoid, sericite, and a few other minerals of negligible importance. The latter, he says, "are noticed in but small quantities to the extent they might occur as accessory constituents of an igneous rock or as products of regional metamorphism or weathering. . . . Quartz is abundant everywhere except in the very best grades of pyrophyllite." Analyses of specimens from several deposits are listed in Table 1, showing that the silica content varies from 57 to 73 per cent and the alumina from 22 to 33 per cent. Oxides of iron and the alkaline metals are collectively present, with one exception, to an extent of about 1 to 1.5 per cent. SOURCES At present, North Carolina is the only commercial source of pyrophyllite, although the mineral has been found in small quantities in many parts of the world. The North Carolina deposits are in the "Carolina Slate Belt," which traverses the center of the state in a southwesterly direction. This

Jan 1, 1940

Receipts General Funds: Initiation fees ' 6,008.50 Arrears of dues 1,772.69 Current dues 46,576.56 Advance dues 1,820.97 Sale of binding 10,554.43 Sale of advertising 6,003.42 Sale of Transactions 3,237.07 Sale of special editions ' 1,722.50 Sale of Bulletins and. pamphlets ' 2,263.95 Miscellaneous Receipts; Interest on investments and deposits 450.06 Sale of pins and fobs 312.80 For the collection of checks 161.84 From Finance Committee, Feb., 1916, Meeting 101.02. Subscriptions to the land fund 86.14 Arizona Meeting refund from N. Y. Central Railroad.. 52.48 Local Section refund from N. Y. Central Railroad.... 31.85 Miscellaneous 425.68 Total Receipts General Funds 81,611.96 Cash balance Dec. 31, 1913 1,063.39 $82,675.35

Jan 2, 1917

By Fred Bond

This paper is a continuation of two earlier papers,1,2 and presents new data on the grindability of various ores and other materials-the results of several years of intermittent research work on the nature of grinding and interpretation of test results. It is divided into five parts: 1. The tabulated results of several hundred grindability tests on a wide variety of ores. 2. A method of correcting screen analyses and calculating from them the surface and other properties. 3. A description of a. new method of measuring the "surface energy" of in ore by pendulum impact tests. 4. Test results. 5. A general discussion of the test results and their application to grinding problems.

Jan 1, 1938

By M. H. Mueller, P. A. Beck, W. P. Chernock

HARRIS introduced the term inverse pole figure for the diagrams previously used by Barrett' to represent the volume fraction p(a,ß) of material in various orientations with respect to the fiber axis in a specimen with fiber texture. The direction of the fiber axis with respect to the crystal lattice is specified by the two independent angle variables a and ß. In such a diagram p gives the fiber axis density distribution over the various crystallographic directions. The p(a,ß) may be given in a two-dimensional diagram by means of contour lines (p=con-stant) in a stereographic projection. The inverse pole figure incorporates in a single contour line diagram all the information given conventionally in pole charts for various (hkl) reflections and, therefore, it represents a considerable degree of condensation. Also, it gives this information directly in terms of the volume fraction of the specimen in various orientations, and it obviates the necessity of referring back and forth between the various pole charts in an attempt to interpret them in terms of orientations. Inverse pole figures undoubtedly represent the most adequate method for describing a texture in a quantitative manner and, at least in the case of fiber textures, this method is certainly a practicable one. Harris described1 a simple procedure for determining at least the rough outlines of a quantitative inverse pole figure. This method depends on the measurement of the intensity of X-ray reflections from various (hkl) planes lying parallel to the same specimen surface. In the case of a rod, reflections from a plane specimen surface perpendicular to the rod axis (fiber texture axis) are to be used. Harris has shown that the measured intensities I,,, reflected by crystal planes (hkl), aligned perpendicularly to the fiber axis of a specimen with unknown fiber texture, and the corresponding intensity Iu nkl from a random specimen are related to the p(a,ß) value for the unknown texture by the following equation IAkl/I°Aklw=c/c°.p(a, ß) [1] where C and C° re parameters depending on the crystal imperfections (extinction), surface preparation (e.g., thickness of oxide layer), the absorption coefficient in the specimen, effective line breadth, and instrumental factors. The values of the variables a and ß1 defining the crystal orientation, depend only on the indices hkl of the reflecting plane perpendicular to the fiber axis. Since p, as described by Harris1, is normalized in such a way that upon integration over the total orientation range its mean value is 1, the parameter C/C may be calculated approximately by the summation of Eq. l over all available X-ray reflections hkl, corresponding to a set of discrete orientations (rather than by integration over the complete range of orientations represented by the continuous variables a and ß). From the summation of Eq. 1 1/n SI AKL/I° Akl = C/C. SP(a,ß)/n is obtained where, as stated above 2p(a,ß) =1. n Therefore

Jan 1, 1959

By C. L. Meyers, J. L. Lytton, T. E. Tietz

The recovery of tensile flow stress of 99.995-pct Al and Al-1 pct Mg alloy was investigated using a fractional recovery parameter. Tensile strainirg was conducted at room temperature, and recovery treatments were made in the range from 80° to 200°C. Equal values of fractional flow stress recovery were found to result in equivalent structural states. Identical recovery treatments were found to produce constant values of fractional flow stress re covery, independent of prestrain. The activation energy for recovery of the 99.995-pct A1 between 80" and 200°C was found to be 23,000 +2000 cal per mole, and the activation energy for the Al-1 pct Mg alloy was 27,500 cal per mole. 1 HE degree of recovery of a cold-worked metal may be studied by measuring the changes which take place in any of a number of properties. Some of the properties which have been used by past investigators include X-ray diffraction phenomena, electrical resistivity, hardness, creep strength, elastic limit, and flow stress. Despite the apparent preponderance of such studies, little is known concerning the effect of recovery on the strength of metals except as deduced from changes in various types of hardness measurements. Furthermore, little information is avail- able concerning the effects which specific solute atoms have on the recovery process. Limited studies have indicated that in some cases solid-solution additions greatly decrease the rate of recovery,' whereas in at least the case of magnesium additions to alluminum an increase in the rate has been reported.2 The purpose of this investigation was to determine the effect of a 1 pct Mg addition on the recovery of high-purity aluminum. Because of the particular interest in the effect of solute additions on the recovery behavior as related to mechanical properties, the degree of recovery was evaluated in terms of tensile flow stress. For the purposes of this study, a recovery process shall be defined as any process, short of recrystallization, whereby the properties, of work-hardened metals tend toward their values ill the unstrained state. EXPERIMENTAL PROCEDURE Test Materials. The materials used in this study were a 99.995-3 A1 and an Al-1 pct Mg alloy made from high-purity base metal. The high-purity aluminum contained the following wt pct impurities: 0.001 pct Cu, 0.002 pct Fe, 0.001 pct Si, and 0.0004 pct Mg. The Pil-1 pct Mg alloy contained 0.001 pct Cu, 0.002 pct Fe, 0.003 pct Si, and 0.99 pct Mg. Both materials were obtained in the form of as-rolled 0.125-in.-thick sheets, from the Alcoa Research Laboratories, New Kensington, Penn. Tensile specimens were cut from these sheets with the longitudinal axis in the rolling direction. Both materials were recrystallized in a molten salt bath; the high-purity aluminum at 450° C for 20 min and

Jan 1, 1962

By Terkel Rosenqvist

Few subjects in iron metallurgy and steelmaking have caused so much discussion and have resulted in so many divergent and partly contradictory statements as the theory of the distribution of sulphur between molten iron and slag. An interesting survey of the different points of view is given by Grant and Chipman.1 Grant and Chipman themselves conclude in their paper that, at least in the open hearth and electric steel furnaces, the governing reaction is a simple distribution like: FeS steel ? FeS alas [Ia] and MnS steel ? MnS alas [Ib] They conclude that no significant reaction takes place according to the more classical scheme: FeS steel + CaO slag ? FeOslag + CaS slag [2a] This is the reaction which is regarded by most investigators as the primary sulphur reaction in the blast furnaces, where it is accompanied by the reaction with carbon: FeO slag + C ? Fe + CO [2b] The writer suggests an alternative to the reactions mentioned above. It is the opinion of the writer that the a priori assumption of defined molecular compounds being present in molten steel as well as in molten slag, has retarded rather than promoted a solution of the sulphur problem. As for the constituents of molten steel, it is taking too much for granted to mention the presence of FeS and MnS. If this infers that the melt contains diatomic molecules, the statement must be made that at least such molecules do not exist in the solid state at room temperature. Solid FeS crystallizes in the nickel-arsenide structure, and MnS (high temperature form) in the sodium-chloride structure. In these structures the sulphur is surrounded by six metal neighbors, and no molecular groups can be isolated. When sulphur is dissolved in molten steel, it is expected to maintain the same coordination number as in the solid state. We know that sulphur in steel has a certain chemical potential and a chemical activity which can be expressed by the reaction: S steel + H2 ? H2S where the activity A. is proportional to the ratio PH2S/Ph2. We know also that this activity is influenced by the presence of other constituents. For instance, there is reason to assume that carbon and silicon increase the sulphur activity and manganese decreases it. However, the exact relationship here is scarcely known, and further investigations are needed. Concerning the molten slags, if anything should be assumed a priori it would be that they are composed of ionic rather than molecular parts. There are indications of this in that solid silicates form ionic structures, and molten slags show high electric conductivity and can be electrolyzed.2 It has been claimed by Taylor and Chipman3 that their activity investigations

Jan 1, 1949

By Terkel Rosenqvist

Few subjects in iron metallurgy and steelmaking have caused so much discussion and have resulted in so many divergent and partly contradictory statements as the theory of the distribution of sulphur between molten iron and slag. An interesting survey of the different points of view is given by Grant and Chipman.1 Grant and Chipman themselves conclude in their paper that, at least in the open hearth and electric steel furnaces, the governing reaction is a simple distribution like: FeS steel ? FeS alas [Ia] and MnS steel ? MnS alas [Ib] They conclude that no significant reaction takes place according to the more classical scheme: FeS steel + CaO slag ? FeOslag + CaS slag [2a] This is the reaction which is regarded by most investigators as the primary sulphur reaction in the blast furnaces, where it is accompanied by the reaction with carbon: FeO slag + C ? Fe + CO [2b] The writer suggests an alternative to the reactions mentioned above. It is the opinion of the writer that the a priori assumption of defined molecular compounds being present in molten steel as well as in molten slag, has retarded rather than promoted a solution of the sulphur problem. As for the constituents of molten steel, it is taking too much for granted to mention the presence of FeS and MnS. If this infers that the melt contains diatomic molecules, the statement must be made that at least such molecules do not exist in the solid state at room temperature. Solid FeS crystallizes in the nickel-arsenide structure, and MnS (high temperature form) in the sodium-chloride structure. In these structures the sulphur is surrounded by six metal neighbors, and no molecular groups can be isolated. When sulphur is dissolved in molten steel, it is expected to maintain the same coordination number as in the solid state. We know that sulphur in steel has a certain chemical potential and a chemical activity which can be expressed by the reaction: S steel + H2 ? H2S where the activity A. is proportional to the ratio PH2S/Ph2. We know also that this activity is influenced by the presence of other constituents. For instance, there is reason to assume that carbon and silicon increase the sulphur activity and manganese decreases it. However, the exact relationship here is scarcely known, and further investigations are needed. Concerning the molten slags, if anything should be assumed a priori it would be that they are composed of ionic rather than molecular parts. There are indications of this in that solid silicates form ionic structures, and molten slags show high electric conductivity and can be electrolyzed.2 It has been claimed by Taylor and Chipman3 that their activity investigations

Jan 1, 1949

By O. W. Ellis

BEFORE entering upon a general discussion of the fascinating, but at present rather controversial, subject of gases in copper, the author feels that some attention should be directed to the work which has been carried out on the solubility of gases in metals. The outstanding contributions to our knowledge of this subject have been made by Sieverts and his collaborators(1) t and by Iwasé.(2) Both the German and the Japanese investigators employed apparatus of the same general design in their investigations. Full reference need only be made, therefore, to the German scheme, which is diagrammatically illustrated in Fig. 1. This, to use the words of Sieverts, which he employed in describing his Burette arrangement of apparatus at the 1928 meeting of der Deutschen Gesellschaft fur Metallkunde(1g): shows a diagram of the usual mode of procedure. A quartz flask contains the metal (for high temperatures a highly refractory porcelain FIG. 1.-SIEVERTS' APPARATUS FOR INVESTIGATING SOLUBILITY OF tube is used) and is connected with the rest of GASES IN METALS. the apparatus by means of a stopcock. The other parts consist of a burette divided into 1/10 c.c., a leveling tube, and art adjus-table mercury reservoir. The burette is connected on one side with the gas inlet and on the other side with the absorption flask; the connection can be interrupted by means of suitable taps. Another tap permits the connection of the flask and the Töpler pump. In an experiment the quartz flask is first exhausted and then a meas-ured quantity of gas is let in from the burette. In the first place the volume of the flask when empty is found by calibration with an inert gas. The pressure is read off on the level tube of the burette, and the temperature measured by means of a thermo-couple whose welded junction lies close to the outside of the quartz flask, which is heated in an electric furnace. In several experiments the quantity of absorbed gas was transferred to a burette by means of a pump and measured.

Jan 1, 1932

By P. H. Dudley

The present paper was suggested by the paper read by Mr. R. W. Hunt at the New York Meeting, in February last, on rail-sections (Trans., xvii., p. 778)) in the discussion of which I brought forward some of the facts and observations here stated. Professional duties having prevented me from writing out my part of that discussion in time for its publication in the volume containing Mr. Hunt's paper, I take the opportunity to present it in separate form and greater fulness. The striking features of the series of rail-sections submitted by Mr. Hunt are their shallow heads and heavy bases. In these respects they are quite similar to the section of the 80-1b. rail, which I designed in 1883 to meet the requirements of the traffic of the New York Central and Hudson River Railroad. Before the adoption of the 80-1b. rail, this road had modified its 65-1b. section from a shallow head with rounding sides and quite heavy base to one having a deep head and thin base. All the leading railroads had changed from the earlier sections of steel rails to those having deep heads and thin bases, conforming to the recommendations of the Committee on Rails of the American Society of Civil Engineers. It is but proper to say that the committee's investigations upon the wear of rails were made upon the rails manufactured under a practice quite different from that which obtained after the committee's recommendations were carried into effect. The results in actual service have been contrary to what was expected. Fig. 1 shows my 80-1b. section of 1883. Before designing this rail I had taken, at different times, a series of diagrams of the condition of tracks, with my car, on the New York Central and Hudson River Railroad, all of the New England railroads, and all but one of the trunk lines. My diagrams gave me an opportunity which could not otherwise have been obtained to see the wear of great numbers of sections of rails under widely varying conditions of traffic.

Jan 1, 1890

By R. M. N. Pelloux

This study of aluminum-copper alloys had two aims: 1) To determine the effect of the amount and distribution of a second phase, CuAl2, on the creep-rupture strength, ductility, and fracture characteristics of the alloys. The work of Gemmell and grant' on single-phase aluminum-copper alloys provided a basis for the present study. 2) To attempt to provide a relation between the microstructure and strength of two-phase alloys deformed at comparatively high temperatures (greater than 0.45 T,). The creep behavior of the two-phase magnesium alloys Mg;Ce and Mg-A1, has been treated by Roberts. 9 In work reported by Sully and Hardy4 and by Underwood, Marsh, and Manning~ on A1-Cu two-phase alloys, and also in a portion of the work of Gemmell and grant,' aging took place during the creep tests. 'In the present work, overaged aluminum-copper alloys were subjected to creep deformation at two temperatures, 500 and 700OF. The overaging treatments to produce the precipitate dispersions were performed prior to the test, at temperatures which were the same as the ultimate respective test temperatures. Hence, the present study is concerned with the creep behavior of stable (in contrast to "underaged") two-phase A1-Cu alloys, i.e., alloys in which no depletion of the solid-solution matrix occurred during: creep. MATERIALS AND PROCEDURE A 2 and a 3 pct Cu alloy, supplied by Alcoa, were studied; Table I shows the compositions. The grain size of the specimens, 0.9 to 1.0 mm, was achieved by annealing the machined test bars for 2 hr at 1000°F, followed by furnace-cooling to 900°F, and homogenizing for 4 hr. Both compositions are in the single-phase condition at 900°F. Two types of overaged dispersions, termed "over-aged I" and "overaged 11" were prepared after the grain size and the homogenization anneals. The overaged I alloys were prepared by quenching to room temperature after homogenization, aging at either 500' or 700°F for 72 hr, and air-cooling to room temperature. The overaged I1 alloys were prepared by furnace-cooling after homogenization, to either 500' or 700°F, and holding at the necessary temperature for 72 hr. The times for furnace-cooling from 900°F to 700° and 500°F were, respectively, about 2 and 3.5 hr. The structures of the A1-2 pct Cu alloys are shown in Fig. 1 (overaged I) and in Fig. 2 (overaged 11). A comparison of Figs. 1 and 2 shows that in the overaged I alloys the precipitate particles along the grain boundaries are much more closely spaced and the grain boundaries are straighter than they are in the overaged I1 alloys. Further, the particle size and spacing in the grains are smaller than in the overaged I1 alloys. Microstructures of the A1-3 pct Cu alloys have not been shown; the structures of these alloys differed from those of the A1-2 pct Cu alloys only in that the distribution density of the particles was greater. The creep specimens had a gage section 1 in. long with a diameter of 0.155 to 0.195 in. Before testing, specimens were electropolished in a solution of 100 cc glacial acetic acid, and 30 cc of 60 pct perchloric acid, at 40' to 50°F, at 24 v. The specimens were kept refrigerated prior to testing to avoid precipitation at room temperature. Constant stress creep tests were conducted; the load was applied 75 min after heating of the specimens to test temperature had begun. EXPERIMENTAL RESULTS Creep-Rupture—Fig. 3 shows the log stress-log rupture life plotfor the overaged alloys studied, and also for the underaged A1-2 pct Cu alloy.' At 700°F, the stress-rupture life relationship is nearly independent of both the amount of precipitate (i.e., composition) and of the type of overaging treatment (i.e., precipitate dispersion). At 500°F it is apparent that the increase in rupture life that was ex-

Jan 1, 1960

By J. D. Verhoeven

The effectiue distriblltion coefficient has been Measured in a series of vertical, normal freezing experirtzents with large current densities passing through the solid-liquid interface. The results indicate that the effect of the current on solute redistribution is due to electvotransport in the liquid. The high currents produced extensive mixing in the liquid which was considerably reduced by solidifying in small lubing. Analysis of the convection indicates that it probably vesulls from a horizontal temperature gradient produced by the Joule heating- of the electvic crirver~t. Due to the strong dependence of this convection upon the specimen radius, it is conclnded that only for specit~ens with radii of less than somewhere between 1 and 2 mm wilt electric field freezing be getlerally effec-tire at enhancing the purification of zone-melting experittierats in loe-melting alloys. Experiments on 0.8-mm lubes illustrate some interesting potential applications of this techniqne as a means of solute control on smcrll specimens. In a number of papers published within the last few years'-4 it has been found that passage of large dc currents through the solid-liquid interface of a freezing alloy produces a change in the solute redistribution accompanying the solidification. It had been predicted theoretically by Hucke et al.s and by Pfann and Wagner that such an effect would occur as the result of electrotransport within the liquid boundary layer at the solid-liquid interface. These authors independently derived the following relation between the effective distribution coefficient and the variables of the process: Where k0 is the equilibrium distribution coefficient, V is the mobility of the solute relative to the solvent, E is the electric field intensity, D is the solute diffusion coefficient, R is the rate of interface motion, and 6 is the boundary layer thickness. Both groups of authors show that this equation predicts the possibility of extending the purification ability of zone-melting experiments by the addition of an electric current. However, there are other effects in addition to electro-transport which could be produced by the high dc current and might, perhaps, invalidate the applicability of Eq. [I]. For example, high electric current might affect the interface reaction or perhaps the equilibrium distribution which was assumed to exist at the interface. It was the purpose of this work to determine the applicability of Eq. [I] by systematically investigating a simple system for which all of the necessary parameters were known. It was of particular interest for speculating on the potential usefulness of this technique to determine the maximum practical field intensities obtainable, and the effect of these high fields upon convective mixing in the liquid. The initial work in this study was published in a previous paper3 which will be referred to as I. In that work, a current density of 2000 amps per sq cm was used with specimen diameters of 5 mm. The results gave a qualitative confirmation of Eq. [I.], and also showed that a large amount of convective mixing was produced in the liquid by the current. The present study is an extension of that work to smaller specimen diameters and higher current densities. Two points were overlooked in I and will be emphasized here: a) the value of ko has not been well-established in the Sn-Bi system and b) the observed convection could be due to thermal convection produced from the Joule heating. EVALUATION OF k0 To evaluate Eq. [ I.] it is necessary to know the value of the equilibrium distribution coefficient, k,. Tn I the value of k, was taken as 0.3 from a published phase diagram.7 According to ansen' the best data on the phase boundaries of the Sn-Bi system are those of Davidson.5 The data of Davidson give a k, value ranging from 0.21 to 0.25 for the compositions studied in this work, or an average value of around 0.23. In a recent publication, Rigaud and Tougas'10 determined ko by means of a solidification technique. For an alloy of approximately the same composition as that used in this work they obtained a ko value of 0.39. Hence, there is considerable uncertainty in the value of ko and, consequently, a series of experiments were made to determine k, more accurately.

Jan 1, 1968

By C. Law McCabe, R. G. Hudson

The Knudsen cell has been employed to determine the free energy of formation of Mn7Cs in the temperature range 800" to 950°C. A value of 66,440 cal was found for hH°o for a-manganese. Measurements of the pressure of manganese over a mixed carbide, (Fe,Mn),C, points to a power relationship between aun7cs and N.4,. RECENTLY Kuo and Perssonl have reported that the carbide of manganese which is in equilibrium with graphite at temperatures up to 1100° C is Mn7Ca. There are no published data on the thermo-dynamic properties of this compound. In order to determine the stability of Mn7Ca, it appeared that, by obtaining the pressure of manganese above 8-manganese and also above Mn,C, in equilibrium with graphite, the free energy of formation of Mn7Ca from 8-manganese and graphite could be obtained. In addition, the vapor pressure of manganese, reported by Kelley From data of Bauer and Brunner,' is subject to some uncertainty and further determinations of the vapor pressure of manganese seemed warranted. In this investigation of the pressure of manganese vapor above pure manganese and also above the carbide of manganese in equilibrium with graphite the apparatus used is the Knudsen orifice cell. The same apparatus, experimental procedure, and method of calculating the pressure was used in this investigation as in one previously reported.~ Care was taken to insure that the cells were at constant weight before using them in a run. The manganese charged in the cell was CP grade powder, carbon free, obtained from the Fisher Scientific Co. A spectroscopic analysis of the manganese after appreciable amounts of it had vaporized from the Knudsen cell showed that no element was present in sufficient quantities to contribute to a weighable weight loss or to decrease the vapor pressure of manganese to any appreciable extent. The spectro-graphic analysis was 0.002 pct Cu, 0.05 pct Fe, 0.002 pct Pb, and 0.002 pct Ni. 8-manganesea is the allo-tropic form of manganese which was present in the cell at temperatures used in this investigation. The manganese carbide, Mn,Ca, was made in the following way: In a closed graphite cell manganese powder was added to graphite powder, which was made from graphite rods for spectrographic use. The manganese powder was the same as that described previously; 5 pct excess graphite was added over that required for the formation of Mn7C,. The mixture was heated in a closed graphite cell for approximately 20 hr at 1350°K under vacuum. X-ray analysis revealed that there was no manganese present after this treatment, but that the lines due to Mn,C, were present. In order to prove that there was no volatile carbide of manganese which was effusing out of the cell, the following experiment was performed: A graphite effusion cell containing graphite power, in excess of that to form Mn,C, of a desired amount, was brought to constant weight on heating at 1228°K. The required amount of manganese was accurately weighed and then added to the graphite effusion cell. The cell was placed in a vacuum at 1228°K for one week, which was the time calculated for the manganese to have effused completely, assuming instantaneous formation of Mn,C8. The cell was then weighed again. This experiment was carried out on two different occasions and both times the weight loss of the cell came within 1 pct of the weight of manganese originally charged minus the weight of manganese left in the cell, as determined by chemical analysis. These data are summarized in Table I. This agreement is considered to be within experimental error and is taken as proof that no carbide of manganese is volatile in this temperature range. It was established, by X-ray analysis, that Mn,C, formed before appreciable amounts of manganese vaporized from the metal powder which was charged. The identification of the carbide of manganese which was present in the Knudsen cell in equilibrium with graphite and manganese vapor was carried out by Kehsin Kuo at the University of Uppsala. He established that the authors' sample, which was submitted to him for analysis, contained the phase

Jan 1, 1958

By Bryan J. Travis, Thomas L. Cook

INTRODUCTION Our growing concern for adequate and secure sources of energy and minerals has stimulated vigorous exploration for new sources, research toward a better understanding of geological processes, and development of new extraction technologies. The need for control, or at least prediction, of subsurface fluid flow is important for many of these technologies for example: primary, secondary and tertiary recovery of oil; ground water and waste management; in-situ fossil energy extraction (oil shale, coal, tar sands); and solution mining of uranium, copper and other minerals. These technologies, especially the last two, are characterized by highly complex systems. A partial list of the physical processes occurring would include flow in porous/fractured media, multi-phase and multi-component flow with heat transport, chemically active fluids and soils, tracers, diffusion and dispersion, fracturing and dissolution. A great deal of understanding of how these processes behave and interact can be obtained from models. MODELS Theoretical models are valuable because they: 1) provide a frame of reference for interpreting results of laboratory and field experiments; 2) once validated by experiments, allow a variety of geometries, injection/production strategies, etc., to be examined (at relatively low cost) for efficiency and stability; 3) can provide guidance to the design of experiments and field operations. Most models are based on the fundamental principles of mass, momentum and energy balance. But from this starting point, many paths can be taken. For example, there is the theory of Payatakes (1973) which concentrates on the microscale dynamics. In this approach, the rock or soil matrix is represented by a complex of characteristic channels (such as periodically constricted smooth tubes). Detail of flow within the characteristic channel is calculated very accurately. A difficulty with this model is that description of a representative channel can require several parameters which may not be easily measured. Also, it is not clear how the channels can be combined practically to model a large scale flow. Another type of model is the "global" one described by Bear (1972). Here, the continuum equations for conservation of mass, momentum and energy are averaged over a distribution of pore channels, resulting in a set of conservation equations in which the small scale structure of the medium is replaced by quantities such as porosity, permeability, dispersion coefficients and tortuosity. This approach allows computation of large scale flows. However, additional constitutive equations are needed which relate averaged quantities such as permeability to observables such as local saturation, particle size distributions, and others. An important difference between models is the way they handle the momentum equation. Payatakes' model solves the full equation. In others, it is replaced by a simpler relation such as Darcy's law (valid for slow flow rates) or by Forchheimer's equation which extends Darcy's law to higher flow rates. These simple relations can nevertheless match a great deal of experimental data (Dullien 1975). The permeability term which appears in Darcy's law and in Forchheimer's expression has been related to other quantities such as porosity and particle surface area. The Kozeny-Carmen equation is a well-known example, valid for some ranges of porosity and particle sizes and for some materials. Several other semi-theoretical, semi-empirical formulations have been devised, none of which are entirely satisfactory. One goal of researchers has been the ability to predict permeability of a porous material from basic measurable quantities such as grain size distributions without recourse to adjustable parameters. This effort has proceeded from consideration of distributions of idealized, non-intersecting channels, to intersecting channels, to consideration of both distributed pore radii and pore neck radii. This last approach has been used successfully to predict permeabilities (ranging over several orders of magnitude) in sandstones (Dullien 1975). Additionally, studies on explicit networks of channels (e.g., Fatt 1956) and percolation theory (e.g., Larson et. al. 1981) have been used to examine interconnectivity effects in porous media with the hope of eventually being able to predict permeability accurately. To be of more than theoretical interest, a model must be compared s controlled laboratory conditions where boundary and initial conditions and relevant material properties can be accurately determined. Also, extraneous forces can be eliminated so that the interactions between processes of interest can be clearly seen and flow models can be vigorously tested. In contrast to the well-defined environment and

Jan 1, 1982

By L. A. Panek

During the past three years, USBM has developed an apparatus and technique for direct measurement of existing pressure and change of pressure in mine rock. This relatively simple and inexpensive monitor is reliable for months after being installed. It is used to determine shift of ground pressure created by different sequences of mining, to ascertain the cause of rock failures, and to evaluate the need for artificial support. The technique has been employed to measure pressures in limestone, greywacke, concrete, diabase, and soft iron ore. When rock is subjected to a load it is deformed. Ordinarily this is observed in a mine as the displacement of one point with respect to another—the deflection of the roof, which may be observed as a convergence between roof and floor; or the extrusion of material from the rib, which may be observed as a decrease of the distance between the rib and the post of a timber set. The effect of excessive pressure may be a rockburst if the rock is strong, or it may be squeezing ground if the rock is soft. Some desirable effects of high stress (high in relation to strength) are the caving of roof in a longwall mining operation, the caving of ore in block caving, and the decrease in mechanical energy required to break down the mineral seam in a retreating pillar-robbing operation. In any case, whether the observable effect of rock load is desirable or undesirable, it is a displacement, and depends on the following four factors: 1) The structure—the size and shape of openings, pillars, and linings, the geologic bedding and jointing. 2) The mechanical properties of the rock—prin-cipally the strength, modulus of elasticity, and flow characteristics. 3) The load or applied stress—primary sources are the weight of superincumbent rock, which increases with depth, and unrelieved tectonic stresses; secondary sources are redistributed pressures caused by other nearby openings, especially large mined out zones (rock pressure depends partly on the rock structure created by mining). 4) Duration of load, related to the length of time the opening is exposed. CONTROL OF ROCK DISPLACEMENT Rock displacement can be controlled by control of these four factors. Consider now the means of exercising such control over these factors. Control of the structural features is obviously possible to a great extent, as such control is exercised largely by choosing the method of mining and the methods of natural and artificial support. Rock properties vary, even within a particular mine, but they are controllable only in the limited sense that control may be exercised by choosing the beds or zones to be mined so that rocks with undesirable properties will not occupy critical positions within the rock structure created by mining. Rock pressure is the most complex of the four factors through which ground control can be achieved because it is invisible, difficult to measure, and poorly understood. Rock pressure is controllable only to the extent that control is exercised on the rock structure created by mining. Considering openings within a particular mine, time of exposure varies, and is readily controllable because it is easily measured and easily understood — the longer an opening stands, the greater the likelihood of failure or excessive convergence. Control is exercised by choice of an appropriate sequence of driving openings of different classes, such as haul-ageways and rooms, which are required to remain well supported for different lengths of time under different conditions. Again, control is exercised through the method of mining. All controllable factors can be controlled by proper design of the mining method. The orientation and relative positions of the mine workings and the sequence of their excavation are likely to be much more important to ground control than is the design of artificial support. This implies that the major decisions in regard to ground control are made, knowingly or not, at the time the mining method is chosen. WHY MEASURE ROCK PRESSURE In addition to restrictions on the several factors, control implies the measurement of these factors in some sense, whether only qualitatively by visual observation, or by actual quantitative determination with a measuring instrument. Rock pressure is the most difficult of these factors to measure, largely because of the interaction between the measuring device and the rock. Nevertheless, the quantitative

Jan 1, 1961