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By W. Kauenhowen

The production of petroleum in Germany during 1932 totaled about 1,608,558 bbl., a slight increase over the 1, 602,517 bbl. produced in 1931. A decline, as shown in Table 1, occurred chiefly in the Volkenroda (Thuringia) field. The total production of the other fields (salt domes), however. reached a new record, about 21 per cent above 1931. Table 1.—Oil Production of Germany by Fields and Oil Provinces, 1928-1932 (Barrels of 42 Gallons)" Salt Dome Province __________________________________________________|_________________________________________________________________________________________________________________________ 1928 274,323 322,742 679 46,319 644,021 644,315 1929 310,891 337,582 10,535 67,578 719,901 720,069 1930 586,404 427,539 100,716 72,485 1,186,969 29,806 1,220,296 1931 506,548 403,634 213,549 116,088 1,242,598 360,885 1,602,517 1932 769,405 366,982 230 979 130,711 1,498,077 110,481 1,608,558 " Official figures published in Germany are given in metric tons. For the above conversion into barrels a factor of 1 metric ton equaling 7 barrels has been used. Includes a very small production from Hcide, Holstein. c Includes a very small production from Tegernsee, Bavaria, and Bruchsal, Baden. Nienhagen-Hanigsen Field In 1932 the Nienhagen-Hanigsen yielded about 51 per cent of the production from the four German salt dome fields. During 1932 the productive area was again extended, chiefly towards the northwest in the so-called north district, to which the present drilling activity is confined almost entirely. Since the discovery of the north district in 1928, about 45 wells have been drilled in it, of which only two were

Jan 1, 1933

By G. R. Speich

A cellular precipitation reaction in which cells consisting of an Ni3Ti (DO24) phase and austenite are formed has been studied in an austenitic Fe-30 Ni-6 Ti alloy. The variation of the growth rate and interlamellar spacing of the Ni3Ti cells with temperature has been determined m the range 400" to 975°C; the interlamellar spacing is proportional to the degree of undercooling; the growth rate can be expressed by an equation of the form G = K?T)2 exp(-Q/RT). The habit of the Ni3Ti lamellae is (001)Ni3Ti (111)y;[010]Ni3T2 [010]y. An almost perfectly coherent interface is formed between Ni3Ti lamellae with this orientation rela -tionship and the intervening austenite. This first Ni3Ti cellular product is subsequently consumed by a second cellular reaction of much coarser spacing. CELLULAR precipitation reactions have been studied in copper-base,1,2 Au-Ni,3 pb-sn,4 and iron-base ferritic5,6 solid solutions, and this mode of precipitation has been treated theoretically by smith," Turnbull,8,9 cahn,10 and more recently by bohm.11 In the case of substitutional austenitic iron-base alloys little or no data are available, Cellular precipitation reactions are well known in austenitic nickel-base alloys12,13 but usually these reactions do not proceed to completion because of general precipitation occurring in the matrix, and they have not been studied in detail. Precipitation from an austenitic Fe-30 Ni-6 Ti alloy was studied as part of a larger investigation of the mechanisms of precipitation from substitutional iron-base alloys. This alloy, austenitic at high temperatures, decomposes at lower temperatures by a double cellular precipitation reaction. The first decomposition product consists of alternate lamellae of an Ni3Ti(DO24) phase and austenite. The reaction proceeds to completion, consuming all of the original austenite. This first cellular product is subsequently consumed by a second cellular reaction of much coarser spacing. The first cellular reaction was studied in detail by light and electron microscopy, hardness measurements, and by X-ray and electron diffraction. Interlamellar spacings and growth rates were measured during isothermal aging in the range 400" to 975°C. The orientation relationship between the Ni3Ti and austenite lamellae was determined and indicates that an almost perfectly coherent interface exists between the two phases. This first Ni3Ti cellular reaction is of particular interest because it occurs over such a wide temperature interval. This allows cellular growth rates and interlamellar spacing data to be obtained for much larger degrees of undercooling than reported hitherto. MATERIALS AND EXPERIMENTAL PROCEDURE The Fe-30 Ni-6 Ti alloy was prepared from electrolytic iron, Mond nickel shot, and sponge-purity titanium* by vacuum melting in a zirconia crucible

Jan 1, 1963

By Donald W. Scott, L. A. Roe, B. J. Sweo

INTRODUCTION THIS paper describes the application of ore-dressing methods to the reclamation of milled frit from over-spray, or waste, porcelain enamel. Frit is the name given by enamelers to a granulated glass produced by the smelting and subsequent water quenching of various ingredients capable of forming a glass, usually including a compound to produce opacity. It is the major component of porcelain enamel, and normally commands a price ranging from 7 to 12 cents a pound. In the preparation of a white enamel slip, usually 6 or 7 parts of clay, 2 parts of opacifier, small amounts of electrolytes, in some cases inorganic color stabilizers and organic dyes, and 35 parts of water are added to loo parts of frit; the mixture then is milled to a fineness of the order of 92 to 95 pct through a 200-mesh sieve. The frit forms the base of the enamel; the opacifier imparts opacity or reflectance; the clay suspends the frit while in slip form and serves as a binder' in bisque form (dry and unfired); and the electrolytes control the workability. Spraying is used commercially, in many cases, to apply the finish coat of enamel to the ware, prior to drying and firing. In the spraying operation, only about 50 pct, by dry weight, of the enamel slip adheres to the surface of the ware, the remainder forms the over-spray. From 1/2 to 2/3 of the overspray goes up the flue where it is lost or recovered, depending on whether the plant is equipped with a dust-collecting installation; the coarser portion of the overspray is collected in the spray booth. The former product is termed flue reclaim enamel, and the latter booth reclaim enamel. Although the spraying operation is done in specially constructed booths, which are partially or completely enclosed, it is extremely difficult to keep out contaminating dirt, which joins the reclaim. Some present-day large enameling plants use 20 tons of frit a day, of which 10 tons go into reclaim with a potential value of $1400 to $2400. When two-coat finish enamels were common, the reclaim was used satisfactorily for the undercoat, but the relatively recent advent of one-coat finish enamels prevented use of the reclaim because, even when blended with first-run enamels, it gave dirty finishes with poor gloss. It was thought that the pitting and specking encountered with reclaimed enamels were caused by the contaminating dirt, and that the poor gloss was caused, primarily, by the high clay content; more clay usually was added to give proper suspension properties to the slip when the reclaim was used. A clay content in excess of about 10 pct usually imparted refractoriness to porcelain enamels. Present-day one-coat porcelain enamels must combine high gloss and opacity with freedom from surface defects. Methods of beneficiating the over-spray,

Jan 1, 1947

By J. Leja, A. Pomianowski

This paper deals with equimolar solutions of xanthate and alkyl trimethyl ammonium bromide adsorption on copper, nickel and sphalerite powders. After an exposition of the experimental methods used and the results obtained, a thorough discussion leads to the conclusion that some molecular association between xanthates and CnTAB's does take place in the bulk of the solution as well as at the air/liquid interface. A spectrophotometric study of xanthate solutions alone and their mixtures with equimolar amounts of alkyl trimethyl ammonium bromide (CnTAB) has established the additivity of ultraviolet spectra (190 to 400 mµ) for potassium ethyl xanthate (KEtX) and C12TAB. No obvious effect of C12TAB addition on the decomposition rate of KEtX was observed, the half life of which was established as 29±3 days at 22°C and pH ~ 6. In mixed solutions of longer xanthate homologues (e.g. hexyl and nonyl) and equimolar CnTAB, colloidal precipitates are gradually formed which contain primarily the corresponding xanthate molecules. The kinetics of collector abstraction by copper, nickel and sphalerite powders were studied in 10-5 to 10"3 M solutions of KEtX alone and in equimolar mixtures of KEtX and CI2TAB. Presence of C12TAB caused a two to three fold increase in the amounts of xanthate (equivalent to many monolayers) abstracted by copper and nickel powders (and in their rates of abstraction) but had no effect on the abstraction of xanthate by unactivated sphalerite (equivalent to less than a monolayer). The adsorption of C12TAB itself from the mixed solutions was very low, at most one monolayer only, and was not influenced by the nature of the solid powder used. A change in the rates of abstraction, observed with copper powder, was interpreted as a completion of a multilayer coating (completely enveloping the grains of powder) following which the rate of reaction between solution and substrate becomes controlled by diffusion through this coating. Work of Buckenham and Schulmanl on molecular associations between different collectors has shown unusual synergistic effects in flotation of individual minerals using mixtures of xanthates and alkyl trimethyl ammonium bromides. The objectives of the present work were: 1) to determine whether these molecular associations between the two types of collectors (indicated by strong surface tension lowering in Buckenham and Schulman's work) take place at the air/liquid interface only or in the bulk of solution as well 2) to establish whether different solids adsorb any species from the mixture of these amphipatic molecules preferentially or as molecular complexes 3) to establish whether there are any differences in the kinetics of adsorption. Metallic copper and sphalerite powder were chosen as adsorbents since they represent two extremes since copper readily adsorbs multilayers of xanthate (and is easily floated with ethyl xanthate) while unactivated sphalerite does not appreciably adsorb xanthate but is known to be readily floated by the amine type collectors. Metallic nickel was included because the infrared spectroscopic work2 on xanthate

Jan 1, 1964

By J. B. Hess, R. L. Dietrich

In the mechanical twinning of magnesium on the {1012} planes the crystal-lographic deformation is such that, in the direction of the hexagonal axis [0001], twinning is possible only undef tension stress, while in the directions perpendicular to the hexagonal axis, twinning is possible only under applied compression. Thus in extruded magnesium and magnesium alloys where the extruded textures are best described as either [1010] or [1120] fibers,' the basal planes are all nearly parallel to the extrusion axis and such material is susceptible to ( 1or2 ) twinning by compression in the direction of the extrusion axis. In order to explain the results of cyclic stressing in alternate tension and compression upon the tangent elastic modulus in such material, Dorn and Thomsen2 have postulated that, following twinning under applied compression, a retwinning or un-twinning occurs as a result of residual microtensile stresses immediately upon removal of the applied compressive force. Recently, Carapella and Shaw4 have used this supposition of untwinning in magnesium in discussing their results on indentation hardness and on cold drawing of MI sheet. In trying to confirm this hypothesis by suitable direct experiments, the authors have been unsuccessful in detecting any evidence whatsoever that untwinning follows the release of applied compression and are forced to conclude that this hypothesis is improbable or, at least, that the quantity of material involved is small. For the experiments, small cylindrical specimens 0.040-in. diam. X 0.120- to 0.140-in. long were etched from 0.0625-in. extruded rod. The ends of the specimens were accurately faced off parallel in a jeweler's lathe. The compression jig was simply an ordinary set of micrometer calipers with an anvil interposed between the spindle and the specimen. The anvil was free to move axially but restrained from rotating so that the rotation of the spindle would not introduce a twisting stress on the specimen. With this arrangement the compressive strains could be estimated to 0.0001 in. and X ray pinhole photographs could be taken with or without load as required. Fig I is the pattern of an uncompressed specimen of AZ3I alloy, showing the approximate [1010] extrusion fiber. The X ray beam is normal to the extrusion axis; in this position it is particularly sensitive in detecting twinning if one directs his attention to the diffraction ring from the basal plane. Since twinning on (1072 planes produced an 86" reorientation of the crystal lattice, the original basal reflections occur at the 3 and 9 o'clock positions while the (0002) reflections from any twinned material will occur at the 6 and 12 o'clock positions. Fig 2 shows the same specimen compressed 3.0 pct, photographed while still under load. This strain has been just enough to produce a detectible amount of twinning and the sensitivity is roughly indicated by the fact that no alterations were produced in the intensities or maxima of the other diffraction rings. A strain of

Jan 1, 1949

By Maurice Rey, H. Beavers

THROUGH circumstances connected with the war, the senior author lost his records, therefore it has been impossible to include numerical data in this paper. The arsenical quicksilver ore investigated had been roasted, with poor metallurgical results. The vapor-tension temperature curves of mercury and arsenious trioxide are similar, and the arsenical compound hampers the coalescence of mercury drops in the condenser and is the cause of large stack losses. The ore was a gray limestone carrying small amounts of carbon and mineralized with cinnabar and two arsenic minerals, realgar (As2S2) and arsenopyrite (FeAsS). The proportion of realgar often exceeded that of cinnabar; the proportion of arsenopyrite was smaller. The grade of the ore varied between 0.8 and 4 per cent Hg. The problem was to make a high-grade mercury concentrate, as free from arsenic as possible. The water used throughout the testing was hard, having a pH of about 8. FLOTATION OF REALGAR Realgar showed a very strong tendency to float. It formed a film at the surface of the pulp and floated in abundance with only pine oil. Therefore an attempt was made to float the realgar before the cinnabar, but this was not very successful; the percentage of mercury in the realgar concentrate could never be brought below 2 or 3 per cent. Cinnabar slimed easily and floated with pine oil, so that some of it always accompanied the realgar. There was also the question of the cinnabar-arsenopyrite separation. On further investigation it was found that realgar can be floated not only with pine oil but even better with a combination of hydrocarbons and pine oil. Washing the ore with ether revealed that it contained hydrocarbons, which helped to float the realgar. In this connection it belongs to the same class as carbon, sulphur and talc. It can be floated also with a xanthate, when activated by a heavy-metal salt. The conditions favoring the two types of flotation are opposed, as activation by a copper salt facilitates xanthate flotation (in fact, is even necessary to it), whereas it hinders pine oil and petroleum flotation. One type of flotation can be termed nonpolar and the other polar, a distinction that has been stressed in a previous paper.1 DEPRESSION OF REALGAR AND FLOTATION OF CINNABAR 'Many chemicals were tested in an attempt to float the cinnabar and depress the realgar. Finally starch rendered soluble with caustic soda was tried, also several grades of commercial soluble starch, and dextrin was found to be the best and the most convenient reagent. Several of these starch preparations have a strong flocculating effect on the pulp, which is a distinct disadvantage. Dextrin, with its low flocculating power, is excellent. It is noteworthy that starch preparations are also depressants for carbon and talc, so that the fact apparently has a general

Jan 1, 1941

By B. Blumenthal

THE present investigation was planned as a survey of the lead-rich portion of the ternary lead-antimony-silver system by thermal analysis. Since, however, a rigorous application of the conventional thermal analytical method is time consuming, an attempt was made to speed up the investigation by reducing the time required for a single thermal analysis. This was done by increasing the rate of cooling to 12° to 18°C. per minute, since such a rate does not permit even an approach to equilibrium conditions, the melt was stirred vigorously by a stirrer operating at the high rate of 665 r.p.m. This proved to be effective in obtaining cooling curves with distinct points of arrest and of excellent reproducibility, which satisfactorily compare with those obtained at a rate of 1" to 2°C. per min. with or without slow stirring (Fig. I). By this method the lead-rich end of the lead-alltimony system and a series of ternary alloys in sections parallel to the lead-antimony side of the ternary system were investigated and it was observed that the two branches of the liquidus curve of the binary alloys did not intersect at the euteotic temperature. An equivalent effect mas observed in the ternary system. The eutectic temperature of the binary lead-antimony system was found to be 252.0°C., which confirms the recent in- vestigation by Pellini and Rhines,1 who determined the eutectic temperature to be 2 51.5°C. The observation that the curves of primarY crystallization of the lead-antimony system do not intersect at the eutectic temperature was previously made by Dean.2 Dean explains the phenomeilon by assuming the existence of a compound Sb4pb. He felt that supercooling was not the cause of the phenomena because he was unable to influence them by inoculation. The X-ray investigation by Solomon and Morris-Jones,3 the metallographic investigations by Stead,4 Charpy,5 Gontermann,6 and Dean, Zickrick and Nix,7 and the numerous investigations of physical properties, definitely disprove the occurrence of any compound. The work of Dean was not confirmed by Broniewski and Sliwoski,8 whose experiments did not show any irregularity and who report a eutectic composition of 13 per cent antimony and a eutectic temperature Of 2500 to 252°C. at a rate Of coo1ing of about 6°C. Per min. Abell Redlich and Adler9 then report a eutectic composition of 12.1 per cent upon reviewing the previous publications and adding a few of their own cooling curves. In 1934 Quadrat and Jiriste10 found from careful analyses of the bottom portion of slowly cooled hypereutectic melts that the eutectic only 11 .4 to 11.5 per cent antimany. (Previous analyses by Stead4 .in 1891 gave 13 per cent.) Weaver,ll however, reported in 1935 that cooling cunres indi-

Jan 1, 1944

By B. Blumenthal

THE present investigation was planned as a survey of the lead-rich portion of the ternary lead-antimony-silver system by thermal analysis. Since, however, a rigorous application of the conventional thermal analytical method is time consuming, an attempt was made to speed up the investigation by reducing the time required for a single thermal analysis. This was done by increasing the rate of cooling to 12° to 18°C. per minute, since such a rate does not permit even an approach to equilibrium conditions, the melt was stirred vigorously by a stirrer operating at the high rate of 665 r.p.m. This proved to be effective in obtaining cooling curves with distinct points of arrest and of excellent reproducibility, which satisfactorily compare with those obtained at a rate of 1" to 2°C. per min. with or without slow stirring (Fig. I). By this method the lead-rich end of the lead-alltimony system and a series of ternary alloys in sections parallel to the lead-antimony side of the ternary system were investigated and it was observed that the two branches of the liquidus curve of the binary alloys did not intersect at the euteotic temperature. An equivalent effect mas observed in the ternary system. The eutectic temperature of the binary lead-antimony system was found to be 252.0°C., which confirms the recent in- vestigation by Pellini and Rhines,1 who determined the eutectic temperature to be 2 51.5°C. The observation that the curves of primarY crystallization of the lead-antimony system do not intersect at the eutectic temperature was previously made by Dean.2 Dean explains the phenomeilon by assuming the existence of a compound Sb4pb. He felt that supercooling was not the cause of the phenomena because he was unable to influence them by inoculation. The X-ray investigation by Solomon and Morris-Jones,3 the metallographic investigations by Stead,4 Charpy,5 Gontermann,6 and Dean, Zickrick and Nix,7 and the numerous investigations of physical properties, definitely disprove the occurrence of any compound. The work of Dean was not confirmed by Broniewski and Sliwoski,8 whose experiments did not show any irregularity and who report a eutectic composition of 13 per cent antimony and a eutectic temperature Of 2500 to 252°C. at a rate Of coo1ing of about 6°C. Per min. Abell Redlich and Adler9 then report a eutectic composition of 12.1 per cent upon reviewing the previous publications and adding a few of their own cooling curves. In 1934 Quadrat and Jiriste10 found from careful analyses of the bottom portion of slowly cooled hypereutectic melts that the eutectic only 11 .4 to 11.5 per cent antimany. (Previous analyses by Stead4 .in 1891 gave 13 per cent.) Weaver,ll however, reported in 1935 that cooling cunres indi-

Jan 1, 1944

By F. H. Wilson, E. W. Palmer

G. L. Bailey (British Non-Ferrous Metals Research Association, London, England)—I was glad to see this further work on the structure and properties of the Cu-Ni-Fe alloys of low nickel content in which we have been so interested in the United Kingdom since before the war." The authors' data on the variation in solubility of iron in both 5 and 10 pct Ni alloys with temperature is based on more detailed observations than we have made but is generally in line with our own work. The difficulty in these matters is in the identification of the structures obtained. The precipitation of the second phase which we presume to be the a' solid solution, richer in nickel and iron, from the a solution with which it is in equilibrium occurs in such a fine state of division that its resolution by ordinary micro-graphic methods is impossible in the early stages. We have published some electron micrographs which illustrate the effects observed more clearly but we agree with the authors when they say that dark staining characteristics when the alloys are subjected to sea-water corrosion are more sensitive in detecting the presence of the a' phase than is the microscope. After taking this point into consideration, however, I confess to some difficulty in understanding Fig. 4. I can only assume that the precipitates visible at such a low magnification as 150 diam in these relatively coarse forms are produced from iron-rich areas of the initial solid solution due to inadequate homogenization. If this is so I find it difficult to accept the authors' contention that such local variations in iron concentration as are capable of giving the heavy precipitates shown in Fig. 4 do not in fact materially affect the solvus surfaces of their equilibrium diagrams. I share the authors' enthusiasm about the resistance to corrosion of these alloys by seawater but I am not fully in agreement with them on the vexing question of the best iron content for these alloys. In Fig. 3 of ref. 8, we give many results showing that the resistance of these alloys to impingement attack in the Jet Test increases as the iron content rises to 2 pct. With higher iron contents pitting at shielded areas is likely to occur. Admittedly the addition of 0.75 pct Fe produces a large improvement in corrosion resistance compared with a pure 90/10 Cu-Ni alloy, but the further improvement on raising the iron to 2 pct is substantial. We recommend from 1.5 to 2 pct Fe as the desirable range from the point of view of corrosion resistance. While it is true that British practice generally uses a hard tube, the corrosion resistance of the 10 pct Ni alloys has in our work been little affected by the structural condition. Although the annealed alloys blacken in seawater, this effect seems to be superficial and not to be accompanied by any real decrease in

Jan 1, 1953

By H. Brevers, Maurice Rey

Through circumstances connected with the war, the senior author lost his records, therefore it has been impossible to include numerical data in this paper. The arsenical quicksilver ore investigated had been roasted, with poor metallurgical results. The vapor-tension temperature curves of mercury and arsenious trioxide are similar, and the arsenical compound hampers the coalescence of mercury drops in the condenser and is the cause of large stack losses. The ore was a gray limestone carrying small amounts of carbon and mineralized with cinnabar and two arsenic minerals, realgar (As2S2) and arsenopyrite (FeAsS). The proportion of realgar often exceeded that of cinnabar; the proportion of arsenopyrite was smaller. The grade of the ore varied between 0.8 and 4 per cent Hg. The problem was to make a high-grade mercury concentrate, as free from arsenic as possible. The water used throughout the testing was hard, having a pH of about 8. Flotation of Realgar Realgar showed a very strong tendency to float. It formed a film at the surface of the pulp and floated in abundance with only pine oil. Therefore an attempt was made to float the realgar before the cinnabar, but this was not very successful; the percentage of mercury in the realgar concentrate could never be brought below 2 or 3 per cent. Cinnabar slimed easily and floated with pine oil, so that some of it always accompanied the realgar. There was also the question of the cinnabar-arseno-pyrite separation. On further investigation it was found that realgar can be floated not only with pine oil but even better with a combination of hydrocarbons and pine oil. Washing the ore with ether revealed that it contained hydrocarbons, which helped to float the realgar. In this connection it belongs to the same class as carbon, sulphur and talc. It can be floated also with a xanthate, when activated by a heavy-metal salt. The conditions favoring the two types of flotation are opposed, as activation by a copper salt facilitates xanthate flotation (in fact, is even necessary to it), whereas it hinders pine oil and petroleum flotation. One type of flotation can be termed non-polar and the other polar, a distinction that has been stressed in a previous paper.' Depression of Realgar and Flotation of Cinnabar Many chemicals were tested in an attempt to float the cinnabar and depress the realgar. Finally starch rendered soluble with caustic soda was tried, also several grades of commercial soluble starch, and dextrin was found to be the best and the most convenient reagent. Several of these starch preparations have a strong flocculating effect on the pulp, which is a distinct disadvantage. Dextrin, with its low flocculating power, is excellent. It is noteworthy that starch preparations are also depressants for carbon and talc, so that the fact apparently has a general

Jan 1, 1943

By Maurice Rey, H. Brevers

Through circumstances connected with the war, the senior author lost his records, therefore it has been impossible to include numerical data in this paper. The arsenical quicksilver ore investigated had been roasted, with poor metallurgical results. The vapor-tension temperature curves of mercury and arsenious trioxide are similar, and the arsenical compound hampers the coalescence of mercury drops in the condenser and is the cause of large stack losses. The ore was a gray limestone carrying small amounts of carbon and mineralized with cinnabar and two arsenic minerals, realgar (As2S2) and arsenopyrite (FeAsS). The proportion of realgar often exceeded that of cinnabar; the proportion of arsenopyrite was smaller. The grade of the ore varied between 0.8 and 4 per cent Hg. The problem was to make a high-grade mercury concentrate, as free from arsenic as possible. The water used throughout the testing was hard, having a pH of about 8. Flotation of Realgar Realgar showed a very strong tendency to float. It formed a film at the surface of the pulp and floated in abundance with only pine oil. Therefore an attempt was made to float the realgar before the cinnabar, but this was not very successful; the percentage of mercury in the realgar concentrate could never be brought below 2 or 3 per cent. Cinnabar slimed easily and floated with pine oil, so that some of it always accompanied the realgar. There was also the question of the cinnabar-arseno-pyrite separation. On further investigation it was found that realgar can be floated not only with pine oil but even better with a combination of hydrocarbons and pine oil. Washing the ore with ether revealed that it contained hydrocarbons, which helped to float the realgar. In this connection it belongs to the same class as carbon, sulphur and talc. It can be floated also with a xanthate, when activated by a heavy-metal salt. The conditions favoring the two types of flotation are opposed, as activation by a copper salt facilitates xanthate flotation (in fact, is even necessary to it), whereas it hinders pine oil and petroleum flotation. One type of flotation can be termed non-polar and the other polar, a distinction that has been stressed in a previous paper.' Depression of Realgar and Flotation of Cinnabar Many chemicals were tested in an attempt to float the cinnabar and depress the realgar. Finally starch rendered soluble with caustic soda was tried, also several grades of commercial soluble starch, and dextrin was found to be the best and the most convenient reagent. Several of these starch preparations have a strong flocculating effect on the pulp, which is a distinct disadvantage. Dextrin, with its low flocculating power, is excellent. It is noteworthy that starch preparations are also depressants for carbon and talc, so that the fact apparently has a general

Jan 1, 1943

By Nelson B. Russell, Donald C. Bond

The effects of various antifreeze agents on the formation of hydrogen sulphide hydrate have been studied. On a molar basis the relative lowering of Tm (the maximum temperature at which solid hydrogen sulphide hydrate can exist in equilibrium with the given solution) for the various agents is: sodium chloride 1.00, calcium chloride 1.71, methyl alcohol 0.57, ethyl alcohol 0.68, ethylene glycol 0.73, diethylene glycol 0.73, sucrose 0.87, dextrose 0.71. On a weight basis the relative lowering of TM is: sodium chloride 1.00, calcium chloride 0.91, methyl alcohol 1.08, ethyl alcohol 0.89, ethylene glycol 0.69, diethylene glycol 0.41, dextrose 0.23, and sucrose 0.15. Introduction The solid hydrate of hydrogen sulphide, H2S.6H20,1 is in equilibrium with water and liquid hydrogen sulphide at 85°F at a partial pressure of hydrogen sulphide approximately equal to the vapor pressure Of hydrogen sulphide at that temperature. At temperatures below 85°F, in the presence Of excess hydrogen sulphide (greater than the amount required to react with the water present) the hydrate is in equilibrium with liquid hydrogen sulphide at approximately the vapor pressure Of hydrogen sulphide. In the presence of excess water, the solid hydrate is in equilibrium with liquid water, containing dissolved hydrogen sulphide, at a pressure lower than the vapor pressure of liquid hydrogen sulphide at the same temperat~re.2 The lower the temperature, the greater the difference between the decomposition pressure of the hydrate and the vapor pressure of liquid hydrogen sulphide at that temperature. Conditions conducive to the formation of solid hydrogen sulphide hydrate may exist in wells producing a gas containing a high percentage of hydrogen sulphide under high pressure, or in the lead lines from such wells. This paper gives the results of tests made with various antifreeze agents which might be useful in decomposing the hydrate or in preventing the formation of the hydrate of hydrogen sulphide Apparatus Fig , shows a diagram of the apparatus used. The sample under observation was contained in a glass tube 34 cm long, having a 6 mm id and a wall thickness of 2.5 mm. The lower end of this tube was closed- with a plug of butyl rubber. The upper end of the tube was connected to a diaphragm gauge, with a stainless steel diaphragm, a manometer, a vacuum pump, and a cylinder of hydrogen sulphide, The tube was held nearly horizontal, with the liquid resting along the lower side of the tube. It was found that when the tube was held in a vertical position, it broke with ex. plosive violence as soon as it became filled with solid hydrate. Presumably this was caused by the expansion which occurred on solidification of the hydrate. The difficulty disappeared when the tube was held in an inclined position during the tests.

Jan 1, 1949

By Maurice Rey, H. Brevers

THROUGH circumstances connected with the war, the senior author lost his records therefore it has been impossible to include numerical data in this paper. The arsenical quicksilver ore investigated had been roasted, with poor metallurgical results. The vapor-tension temperature curves of mercury and arsenious trioxide are similar, and the arsenical compound hampers the coalescence of mercury drops in the condenser and is the cause of large stack losses. The ore was a gray limestone carrying small amounts of carbon and mineralized with cinnabar and two arsenic minerals, realgar (As2S2) and arsenopyrite (FeAsS). The proportion of realgar often exceeded that of cinnabar; the proportion of arsenopyrite was smaller. The grade of the ore varied between 0.8 and 4 per cent Hg. The problem was to make a high-grade mercury concentrate, as free from arsenic as possible. The water used throughout the testing was hard, having a pH- of about 8. FLOTATION OF REALGAR Realgar showed a very strong tendency to float. It formed a film at the surface of the pulp and floated in abundance with only pine oil. Therefore an attempt was made to float the realgar before the cinnabar, but this was not very successful; the percentage of mercury in the realgar concentrate could never be brought below 2 or 3 per cent. Cinnabar slimed easily and floated with pine oil, so that some of it always accompanied the realgar. There was also the question of the cinnabar-arsenopyrite separation. On further investigation it was found that realgar can be floated not only with pine oil but even better with a combination of hydrocarbons and pine oil. Washing the ore with ether revealed that it contained hydrocarbons, which helped to float the realgar. In this connection it belongs to the same class as carbon, sulphur and talc. It can be floated also with a xanthate, when activated by a heavy-metal salt. The conditions favoring the two types of flotation are opposed, as activation by a copper salt facilitates xanthate flotation (in fact, is even necessary to it), whereas it hinders pine oil and petroleum flotation. One type of flotation can be termed nonpolar and the other polar, a distinction that has been stressed in a previous paper. DEPRESSION OF REALGAR AND FLOTATION OF CINNABAR Many chemicals were tested in an attempt to float the cinnabar and depress the realgar. Finally starch rendered soluble with caustic soda was tried, also several grades of commercial soluble starch, and dextrin was found to be the best and the most convenient reagent. Several of these starch preparations have a strong flocculating effect on the pulp, which is a distinct disadvantage. Dextrin, with its low flocculating power, is excellent. It is noteworthy that starch preparations are also depressants for carbon and talc, so that the fact apparently has a general

Jan 1, 1941

By A. L. Engel

IN the treatment of complex ores by flotation, one of the most important steps is conditioning the feed. Conditioning primarily consists of the addition, in the grinding circuit, of an alkaline reagent, for example sodium carbonate, which neutralizes any acidity of ore and mill water, counteracts the effect of 'harmful soluble salts, disperses colloids, and provides the necessary alkalinity for the best metallurgical results. The several minerals of the ore should be put in such condition that they may be floated or rejected as desired, through the action of further reagents thereafter used.

Jan 1, 1932

By Klaus-Peter M. Hanke

INTRODUCTION In early 1979 Jim Walter Resources, Inc. (JWR) of Brookwood, Alabama approached TMCI Construction, Inc (TMCI) to make a proposal on a program that involved the sinking of up to 10 ventilation shafts of approximately 6.7 m (22 ft) diameter and ranging in depth from 500 to 700 m (1650 to 2300 ft) for the JWR coal mines in Alabama. At this time TMCI was already constructing the first spiral underground bunker (capacity 2000 tons) in North America for the JWR organization at their No. 4 mine in Alabama. The TMCI proposal was based on the use of the mos modern large diameter shaft boring machine rather than sinking the shafts using the conventional drill blast-muck technique. The proposal was made based o: the experiences by the parent company, Thyssen Schachtbau, which has been using this type of machin in Germany for shaft boring since 1971. As a result of the TMCI proposal JWR issued a purchase order to TMCI for the construction of four 6.7 m (22 ft) diameter, concrete lined, unfurnished ventilation shafts ranging in depth from 500 to 700 (1650 to 2300 ft). An order was thus placed with WIRTH Machinen- and Bohrgeraete Fabrik GmbH, in Germany for the manufacture of a model 650/850 E/Sch "Schachtbohrmaschine" (Vertical Shaft Borer = V-mole which arrived on site in Alabama in early 1981. The first V-mole GSB 450/500 was introduced in Germany in 1971 and was capable of enlarging in one step a pre-drilled 1.2 m (4 ft) pilot hole to 4.5 - 5.0 m (14.7 - 16.4 ft). This machine has sunk 9 staple shafts and deepened one surface shaft for a total of 2360 m (7740 ft) of shafts. On the last shaft boring operation in 1978 the machine was converted as an experiment to drill without a pilot hol using a hydraulic pumping system to remove the cutting debris. A second generation machine, the SB VI 500/650, was introduced in 1977 for enlarging the pilot hole to a range of 5.0 - 6.5 m (16.4 - 21.3 ft) diameter. This machine is still in operation and has already drilled well over 2000 m (6500 ft) of shaft. The third generation of V-mole, the SB VII 650/85( for diameters from 6.5 to 8.5 m (21.3 to 27.9 ft) was: commissioned in May 1980 and has been used for two surface shaft deepenings totalling 606 m (1990 ft) with another scheduled for 1982. The main advantages favouring the use of such V-moles were identified as: 1) A reduction in manpower to the crew required in a conventional shaft sinking operation. 2) A considerable reduction in time to complete a shaft compared to conventional techniques. 3) The use of the V-mole eliminates many of the hazards encountered in conventional sinking. Based on the successful performance of the first three V-moles in Germany, Thyssen Schachtbau decided to employ this principle abroad. In 1980 a second machine of the third generation was built and is now operated by TMCI Construction, Inc. in Alabama. The first shaft was completed at the end of 1981 and this paper describes the method of operation including some unique aspects not attempted on prior V-mole operations and some of the statistics arising out of the experiences during the first shaft boring operation. THE NO. 7 MINE FAN SHAFT SITE Jim Walter Resources, Inc. was formed in 1970 to exploit the coal field in Alabama on the southern tip of the Appalachian coal field. The coal reserves amount to around 650 million tons of mainly good quality coking coal of which about 350 million tons are to be extracted over the next 30 years. Shaft sinking and preparatory work began in 1972, and at present 6 mines are producing around 5.4 million t.p.a. Annual production is to expand to 10 million t.p.a. as soon as possible, and the ventilation shafts to be sunk by TMCI play a vital role towards attaining this goal. The first shaft site is located at the No.7 mine, near Brookwood, Alabama. The actual location of the shaft relative to the production shafts is shown on the mine plan (Fig. 1), which also shows the room-and-pillar extraction system used at present. The mine plan further shows the conveyor route used for the muck removal. The geological survey showed that the strata consisted of horizontal layers of mainly sandstone, sandy shale and shale interspersed with several coal seams. The seam being extracted at the No. 7 mine is a combined seam made up of the Blue Creek and Mary Lee seams at a depth of 513 m (1682 ft) and having an average seam thickness of about 2 m (6 ft). At the beginning of September 1980 the surface site preparation and pre-grouting work was completed by JWR, and TMCI was able to commence with Stage I of the shaft sinking program - the drilling of the pilot hole.

Jan 1, 1982

By Walter Lang

The year 1931 has shown a marked change over 1930 in New Mexico, with respect to the volume of activities attendant upon the petroleum industry. Although the total production of oil and gas this year exceeds that of preceding years, the results have been attained from established units operating under restriction, but capable of supplying far more than the economic conditions justify. The presidential order of March 12, 1929, that "there will be complete conservation of Government oil in this administration," has merely anticipated a normal consequence of overdevelopment. As a result of the combined economic and legal restrictions imposed, very little new drilling has occurred during the year. Even in proven areas the drilling of offsets has been curtailed to the absolute limit of requirements. Scouting and sample-cutting, which in 1930 were still in a state of feverish activity, are at low ebb, and lease buying has reached a condition of stagnation. A number of the major oil companies have either materially reduced their field and office forces or completely eliminated local office representation. Two tests of particular interest, because correlation shows them to be structurally high although they failed to produce, are the National Securities well drilled six miles west of the town of Hobbs, on sec. 33, T.18 S., R.37 E., Lea County, to a total depth of 4272 ft., which developed a flow of 4,000,000 cu. ft. of gas at 3860 ft., and a show of oil; and the Western Drilling Co. No. 1 State, sec. 16, T.20S., R.32 E., Lea County. The latter test found dead oil at 2575 to 2580 ft., and sulfur water at 2745 ft., increasing to 2780 ft., representing the zone from which production was generally expected. The well was drilled to 4013 feet. The discovery of sulfur at about 950 ft. in the deepening of an old water well (Pearson, NE. 1/4 sec. 8, T.16 S., R.25 E.) drilled in the Little Cottonwood area northwest of Artesia led the Union Sulphur Co. to drill three prospect tests on a block of acreage in the vicinity during the summer and fall. The results of the investigation have not been disclosed. The Kummbaca Oil and Gas Co. drilled the T. J. Kerline No. 1, in sec. 34, T.21 N., R.30 E., Harding County, gaging 3,654,000 cu. ft. of 98 per cent CO² at 940 ft. The Barton structure, 20 miles east of Albu-

Jan 1, 1932

By D. J. Carney, R. L. Stephenson

A sampling technique has been developed for procuring a sample of sinter representative of the entire depth of the sintering bed. The sampling method involves the use of an open-bottom metal basket that rides on the grate of the sintering machine and when removed contains a sample of the sintered product. Additional data have been obtained to indicate that the tumbler test is a suitable means of measuring sinter strength. IN the last few years additional sintering facilities have been installed in both the Pittsburgh and the Chicago district of the United States Steel Co. Since the construction of these sintering plants made possible the use of higher percentages of flue-dust sinter in our blast-furnace burdens, it became important to study means of controlling the quality of sinter to obtain optimum results in the blast furnace. For controlling an operating process, it is necessary first to establish standards by which the quality of the product can be judged. For sinter, it appeared that an important property was its strength or its resistance to degradation during transportation and charging into the furnace. Consequently work was undertaken to establish a standard for sinter strength that could be used both for controlling sintering-plant operations and for correlating sinter quality with blast-furnace performance. The first problem in setting up a standard was that of procuring a sample that would be representative of the sinter made under any particular set of conditions at the sintering plant. Since the United States Steel Co. sintering plants discharge the finished sinter either into a large pit or onto a rotary cooler, the sinter becomes inseparably mixed with material sintered 2 hr before or 2 hr afterwards. For this reason the exact identity of the sinter is lost. A sample selected as the cooler is discharged, or as the sinter is removed from the pit, cannot be said to be truly representative of the sinter made at any specific time. Sampling The first attempt to procure a sample that would be representative of a specific sinter mix and of specific operating conditions was made by stopping the Dwight Lloyd sintering machine and removing an entire pallet full of sinter. This method, however, proved very difficult to perform and interfered considerably with the operation of the plant. To overcome this difficulty, a sampling method was devised by technologists at South Works enabling them to secure, without interrupting the sintering operation, a sample of about 1 cu ft of sinter, representative of sinter for the full depth of the sintering bed. The South Works method involves the use of a steel-frame-work basket. A typical basket is shown in Fig. 1. The basket has been used both with and without crossbars along the bottom. As long as the crossbars are in the same direction as the grate bars on the sintering machine they do not interfere with the sintering process. The basket is set on an empty grate of the Dwight Lloyd sintering machine before it passes under the swinging feed spout, see Fig. 2. When the basket is removed after it has travelled the length of the sintering machine, it contains the sample. Just before the basket is removed, the sinter is scored and chipped to facilitate removal of the sample from the sinter bed. A view of the basket after its removal is shown in Fig. 3. Although the sampling method was originally designed for use on a Dwight Lloyd sintering machine, it can also be used on the Greenawalt type of machine. When used on the Greenawalt-type machine, the basket is placed on the sintering grate before the charging car passes over it, and finally it is removed just before the pan is dumped. Testing After a method of obtaining a representative sample of sinter had been developed, the next step was to select a method of measuring its strength. The irregular shape and size of the sinter pieces precluded the use of a simple compression test for determining strength; consequently, the shatter test and tumbler test were investigated. To perform the shatter test, a sample of sinter, approximately 5 lb, is dropped from a hinged-bottom box at a height of 3 ft onto a steel plate. The broken sinter is sieve-analyzed after a specified number of drops. The tumbler test is performed with the use of a standard ASTM coke-tumbling drum. The drum is 3 ft in diam and is equipped with two lifter bars diametrically opposite one another on the inner periphery of the drum. The drum is rotated at a speed of 24 rpm for 200 revolutions, and after tumbling the sample is sieve-analyzed. To express as single numbers the results of sieve analyses after shattering or tumbling, the method suggested by R. E. Powers1 was employed. This method involved plotting the size of the sieve openings on a logarithmic scale and the cumulative per cent larger than each sieve on a probability scale as described by J. B. Austin.' By interpolating from the plotted data, which in most cases approximated

Jan 1, 1954

By P. S. Rudman

Crystal-structure occurrences in binary phase diagrams of fifth- and sixth-period elements, zirconium through palladium and hafniun through platinum, are surveyed with the conclusion that average .group number GN is the dominant correlative. This is interpreted in terms of curves of enthalpy differences between competitiue structures that are continuous func -tions of GN. It is further reasoned that the absolute formation energies may also be continuous functions of GN and if so can be simply obtained from the regatives of the heats of sublimation of the elements. It is shown that from such a heat of formation-GN plot the heats of mixing of alloy systems can be quantitatively predicted. For example, for sixth-period alloys very large exothermic heats of mixing are predicted for systems that span GN = 6 (i.e., Hf-Pt, Ta-Os, ...). Thermodynamic data with which to test these predictions do not appear to be available. If in the latter transition (A subgroup) elements we eliminate from consideration the fourth period where magnetic terms contribute to crystal-structure stability, as shown in Table I, there is a very regular sequence of structures. Using the group number (GN) assignments of Table I, which differ from the usual assignments of 8 to the elements listed as 8 through 10, it is perhaps trivial to say that the phase occurrence is a unique function of GN. However, the interesting aspect of alloys from among these elements is that the alloy structures also appear to correlate with GN. The GN for an alloy is given as GN = SixiGNi, where xi and GNi = atomic fraction and GN of component i, respectively. It is difficult to credit anyone in particular with having discovered this correlation, so many people have implicitly or explicitly employed it in the last 10 years. However, Bloom and Grant' in their correlation of s-phase occurrence with total number of d + s electrons were certainly one of the first to appreciate the correlation and Hume -Rothery2 appears to be responsible for the use of average GN as defined above. Only in the last few years have the phase diagrams of enough alloy systems been determined for this correlation to be surveyed with any degree of completeness. We shall here, in an abbreviated format, summarize the available phase-diagram literature and discuss some consequences of the GN correlation. BINARY DIAGRAM SURVEY In Figs. 1 to 3 the phase occurrences are summarized. In Fig. 4 the occurrence limits for the more common structures are summarized. That the GN of an alloy falls within the occurrence limits of a particular structure is a necessary but not a sufficient condition for the appearance of that structure. The preceding figures certainly illustrate that GN is a dominant correlative for structures of these elements. Many of the diagrams have complications, with ordering and other phase changes occurring in intermediate phases, that cannot be clearly accommodated in such a schematic survey and have hence been left out. Such omissions cannot, however, negate the GN correlations discussed here. Relative atomic size is also an important crystal-structure determinant and since atomic size varies quite regularly with GN for these elements it is possible that the apparent GN correlation is basically a size correlation. In Fig. 5 relative size occurrence limits are given for intermediate phases and extended terminal solutions. The relative volume, ?v/(v) - 2(vA - vB)/(vA + uB), has been taken as the measure

Jan 1, 1968

By N. F. Fiore, M. C. Mangalick

DISLOCATION damping in single crystals is orientation dependent.&apos; If dislocations are distributed uniformly over all the slip systems in a crystal, and if each dislocation contributes identically to the damping process, then a damping loss or decrement 6 arises. In fact, however, for a crystal of axial direction (hkl), dislocations on certain slip systems are oriented to make a larger contribution to the damping loss than are dislocations on other slip systems. Thus the measuring damping, 6 (hkl) is proportional to an orientation factor (hkl), which weights the ability of each slip system in the crystal to contribute to the total damping. If it is assumed that dislocations are distributed uniformly on all slip systems, then for a given orientation of an fcc crystal this factor is determined2,3 by the three nonzero elastic constants Cll, C12, and C44 and the density p. In this communication measured values of elastic constants for two Fe-18Cr-Ni alloys are reported, and the dislocation damping results on two different orientations of each alloy are analyzed for orientation dependence. Elastic constants were determined by measuring the ultrasonic velocities of one longitudinal and two shear waves in (110) direction of the fcc crystals.4 Variation of velocities with the change in orientation is very small for (110) orientation,3 and so this direction is ideal for orientation factor and comparative damping measurements. Experimental Procedures. The nominal compositions of the alloys studied are given in Table I. These alloys were vacuum-melted and vacuum-cast from high-purity materials at U.S. Steel Applied Research Laboratories. The single crystals were grown by the modified Bridgeman technique. The specimens were homogenized at 1350°C for 20 hr, cut to shape and size with a spark cutter, and then annealed at 1100°C for 20 hr prior to use. In the KHz frequency range, the Marx composite piezoelectric oscillator was used to obtain the damping. The ultrasonic pulse technique was used to measure the ultrasonic velocities and the attenuation in the MHz frequency range. M.c.mANGALICK,-- StudentMemberAIME,formerly Research Assistant, University of Notre Dame, is now with Casting Laboratory, Chase Brass and Copper Co., Cleveland, Ohio. N. F. FIORE, Associate Member AIME, is Assistant Professor, Department of Metallurgical Engineering and Materials Science. University of Notre Dame, Notre Dame, Ind. This communication is part of a Ph.D. thesis presented by M. C. MANGALICK to the Graduate School of the University of Notre Dame. Manuscript submitted May 20. 1968. IMD Elastic Constants. Table I gives the values of the ultrasonic velocities. Values of C11, C12, and C44 calculated from these velocities are also given in Table I, and it is evident that there is very little variation in C11, C12, and C44 with nickel content. This slight variation may be attributed to inaccuracies in velocity measurements and practical differences in the orientations of the specimens. For example, in B the time interval for vl was 2.4 ± 0.05 sec giving an error in v1 of 0.235 x or 0.005 in. per sec. The elastic constants obtained by pulse technique were tested by calculating E<110>, Young&apos;s modulus for the (110) direction, from the equation: This value was compared with the value computed from the resonance bar measurements in which where fr is the resonance frequency and I, is the length of the specimen. In all cases, the values calculated from the ultrasonic velocity measurements

Jan 1, 1969

By RALPH HAYES SWEETSER

ONE per cent. of ash in a ton of coal has been so little considered that in many circles it has been positively ignored. Even P. T. Barnum had never heard of it, or he would have had one on exhibition alongside the Cardiff Giant and the White Elephant. One per cent. of ash is closely related by both those freaks of Barnum in that it is "stone" and, in its aggregate, it is the greatest "White Elephant" that the American public now supports. Some of you may have paid Mr. Barnum for a look at the "petrified man" (named the Cardiff Giant by the gullible wise men of the early seventies); but it is certain that everyone of you is now paying for the support of the great White Elephant that is being constantly carried by our railroads all over the country-at the public&apos;s expense. " One per cent. of ash in a ton of coal" requires 120,000 open-top railroad cars each year to transport this use- less stone giant from its native bed in the coal seams of the bituminous regions to the coal bins of the consuming public.

Jan 1, 1924