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By R. S. Handy

AT THE TIME of my first visit to Bolivia in 1927 the tin-mining industry was prosperous, the tin price at London being more than £300 per long ton of tin, and the operators were making every effort to bring their plants up to the very highest point of capacity as well as of efficiency. Any device or piece of equipment or method that gave promise of increasing production was welcomed regardless of the cost, and the plants were being modernized as rapidly as human ingenuity could make it possible. At the time of my second visit in 1932, however, conditions had changed materially. The price of tin had fallen to a little over £100 but costs had not decreased anywhere in proportion and operators were at their wit's end to cut the operating losses that were everywhere prevalent. Charles L. Bradbury, manager of the Empresa Minera de Huanuni, at Huanuni, Bolivia, had been recently called from Mexico to make all analysis of the situation and to attempt to work out a remedy for the economic conditions that threatened to close the mine. His analysis brought out the following points:

Jan 1, 1938

By T. L. Joseph

S. T. Killian (Johnstown, Pa.)—This is one of the finest papers I have read. Tying in stoichiometric calculations with furnace performance and practice is a step which had to be taken sooner or later. The noteworthy difference between Dr. Joseph's type of calculations and regular blast furnace calculations is that the Ib mol system is used as a basis. With the Ib mol system, weights, volumes, and chemical reactions can all be expressed in the same equation. In the paper, wind, ore, flux, and fuel are all expressed as lb or lb mols. Probably Dr. Joseph does not realize it, but the vague word coke appears only twice in the entire paper. Lb of C and Ib mols of C are followed through reactions but the word coke appears only as 1560 lb coke per ton of pig and 1700 lb of coke per ton of iron. Obviously in order to understand furnace reactions, the coke should be expressed as lb or lb mols of C. Furnaces can also be compared more easily. In some respects the paper is too thorough and too complete. The effects of the metalloids reduced into the iron upon the top gases represents a difference of less than 3 pct of the CO formed in the bosh. Due to the completeness of the calculations in relation to the CO/CO2 ratio, this was included and was necessary. However, the exclusion might have enabled more furnace men to follow the lb mol system of calculations through the blast furnace to a better degree. By considering only irons of similar analysis, this part of the calculations might have been omitted. However, if this had been done, total rewriting of the paper later would have been necessary in order to make the work complete as it is now. It also would not have been nearly as authoritative. In the paper, there appears the reaction: H2O + CO ? CO2 + H2 [I] Dr. Joseph states that he did not take this reaction into consideration in any calculations pertaining directly to the paper. The piobable reason- for this is that although it contains all the main reacting top gases except N2, it is rather inflexible since it is monomolecular in relation to each of the reacting gases and does not tie in with the gasification of C. Actually the reactions: H2O + C ? CO + H2 [2] 2H2O + C ? CO2 + H2 [31 and the solution loss reaction: CO2 + c ? 2c0 [41 tend to assume an equilibrium through the reaction: H2O + CO ? CO2 + H2 [I] which should be considered a balancing or equilibrium reaction. Reactions 2, 3 and 4 permit furnace conditions to balance with the CO/CO2 ratio and H2 formation. They tie in with the solution loss. Reaction 1 unites them chemically. Probably the best calculation to make at this time would be to try to find the relative importance of the CO2 from the flux and the H2 in the dilution on an actual furnace gas analysis. For this purpose the Dob-scha-Carnegie-Illinois paper—"Effect of Sized and Sintered Mesabi Iron Ores On Blast Furnace Performance" is chosen. This paper was presented before the blast furnace section of the AIME in 1948. This represents the best large scale furnace operation available to me. Unfortunately the changes were brought about by beneficiation of the burden and not by changes on one burden. In choosing the basis for the calculation in relation to the furnace, 100 mols of dry top sgas is chosen. This leaves something to be desired inasmuch as the nitrogen basis is changing but I believe it will be better understood than any other type and it is the easiest to use.

Jan 1, 1952

By T. L. Joseph, G. Bitsianes

THE layered structure of partially reduced iron ore was described in a previous paper.' Reduction by hydrogen was found to take place at well-defined interfaces between layers of the solid phases. In the present investigation, a detailed study was made of the wiistite phase that had formed during the partial reduction of a cylindrical compact of chemically pure hematite. An unusually wide band of wiistite permitted a rather detailed study of this phase. The specimen was made from Baker's C.P. hematite in the form of a cylinder 1.5 cm in diameter and 1.8 cm long. A dense ore structure with about 6 pct porosity was attained by heating the specimen in air at 1100°C for 3 hr. To confine reduction to the top surface, a ceramic coating was applied to the bottom and sides of the cylindrical compact. The specimen was then partially reduced in hydrogen at 850°C and subjected to a coordinated sequence of macro-, micro-, and X-ray examinations. A section of the partially reduced cylinder is shown in the macrograph, Fig. 1. Four layers consisting of metallic iron, wustite, magnetite, and unreduced hematite are clearly shown. The effort to force reduction to proceed downward in topochemi-cal fashion was only partly successful, as some reduction occurred along one side and bottom of the cylinder. A rather wide layer of dark wustite phase had formed, however, and permitted sampling for X-ray studies as indicated. To supplement previous work and to study the wustite layer in more detail, ten separate layers were removed for X-ray examination. Broad and diffuse patterns were obtained with the as-filed powders, especially with those of iron and wiistite, and the condition indicated a cold-working and variable composition effect within the respective layers. This condition was corrected by annealing the entire series of powders at an appropriate temperature. For the annealing treatment, the ten powder samples were wrapped in silver foil, sealed under vacuum in small quartz tubes, and heated at 750°C for 16 hr. The specimens were then drastically quenched in cold water to preserve the annealed condition. These annealed specimens were X-rayed in turn and the compiled patterns are shown in Fig. 2. The standard patterns for iron and its oxides have been interjected at appropriate positions for purposes of comparison and phase identification. All of the patterns obtained were clearcut and concise so that positive identifications could be made for all of the phases. The outermost layers A, B, and C were composed almost entirely of iron with a small amount of wiistite being detectable at the X-ray limit of phase detection. Layer D from the iron-wustite interface showed both of these phases. The next four layers E, F, G, and H were all in the dark phase band which had been tentatively identified as wustite by the macroexamination, Fig. 1. The diffraction data with their single-phase patterns of wiistite for these layers checked the visual evidence. Continuing the X-ray analyses after layer H, the macrograph (Fig. 1) shows that layer I came largely from the magnetite zone but included some fringes of the wiistite-magnetite interface. The diffraction pattern for the sample confirmed this observation. Layer J came from the unreduced core of the specimen and its diffraction pattern indicated a preponderance of hematite phase. The reduction behavior of synthetic compacts has thus been found to be similar to natural dense iron ore. The previous results were supplemented with measurements of the diffraction films and calculations of the respective unit parameters. These X-ray data are summarized in Table I and offer some interesting correlations as to the compositions of the various phases undergoing reduction. The iron layers that were analyzed gave lattice parameters close to that of pure iron at 2.8664A. Evidently this iron was present in layers A through D as a pure phase with little or no oxygen dissolved in its lattice. With the wiistite layers an entirely different situation prevailed in that there was a definite and

Jan 1, 1955

By A. F. Meston

Centrifugal force has been used for centuries for separating liquids but machines for doing this are a comparatively recent development. The use of these machines is being extended into many industries but this paper is confined to their use in the oil industry. The centrifugal machine is found at the well where "cut oil" is dehydrated for acceptance by pipe lines; and in the refinery and byproduct plant. In fact, wherever finely divided suspended particles should be removed from an oil, there is a possible use for a centrifugal machine, if the particles have, or can be made to have, a specific gravity different from that of the oil. Centrifugal machines are also used for cleaning fuel and lubricating oils and dehydrating transformer oils. Applications and Results When oil comes from the well mixed with water, it is spoken of as cut oil. Settling often does not remove sufficient water for the oil to be accepted by pipe lines, thus necessitating chemical or other treatment. Centrifuging alone, or following chemical treatment, effectively prepares such oil for pipe lines, as is shown by the following data: WateR, Etc. Wat~R. Etc. Temperature, Oil to Pipe Line, aT StUt at Finish Degrees F. Bel. Per HouR PIE Cent. PEECent Oklahoma lease.... 160 10 10 0.25 Kansas lease....... 125 4 20 0.25 to 2 On the Oklahoma lease, the machine was cleaned of solid material once in 12 hr. At first, it was thought that chemical treatment was necessary to start separation and 1 qt. of prepared compound was added to each 100 bbl. of the cut oil before centrifuging. Later it was found that

Jan 1, 1924

By Walter Bradley

MINING by hydraulic process of the important gold-bearing gravels of the Sacramento Valley in the basins of the Yuba, Bear and American rivers began in 1853, and continued at an ever-increasing rate for 30 years. In its most active days it reached an annual production of $15,000,000, and averaged $10,000,000 per year over the 30 years. During that period no provisions were made to prevent the debris from being dis-charged into the water courses, and ultimately large quantities of silt, sand and gravel were washed down to the lower valleys; filling channels, causing overflow of agricultural lands and difficulty in maintaining navigable depths in the Sacramento River. Agitation and suits filed because of these damages finally resulted in the injunction decision of Judge L. B. Sawyer,1 in the U.S. Circuit Court, Jan. 23, 1884, which closed down practically all hydraulic mining operations not having means to restrain their debris. In 1893 (approved March 1, 1893), Congress passed the act introduced by Representative Anthony Caminetti, of California, creating the California Debris Com-mission, composed of three officers assigned from the Engineer Corps of the U.S. Army, and since that time it has been legal and possible within the drainage systems of Sacramento and San Joaquin rivers to conduct hydraulic mining of gold-bearing gravels behind dams built under this commission's permit and supervision. In the watersheds of the Trinity and Klamath rivers, which flow directly to the Pacific Ocean and do not affect navigation or agriculture, operating permits from the California Debris Commission are not required. There is a measure of restriction there, however,. through what is known as the Trinity and Klamath River Fish and Game Dis-trict. Chap. 215, Stat. 1931, in order to secure relatively clear water for the fishing season, provides that between July 15 and October 15 each year there must not be discharged into these rivers debris that will cause a turbidity greater than a content of 50 parts per million in the

Jan 1, 1936

By Webster Hodge

MALL generators and motors are required to Soperate, in some critical applications, at temperatures where cold-worked silver-bearing copper re-crystallizes. Copper containing up to 30 oz Ag per ton has been used for many years to build the highest grades of commutators and slip rings. With failure of commutators impending because silver-bearing copper cannot withstand the stresses imposed at these higher temperatures, Cr-Cu was tried as a substitute with varying degrees of success. Cr-Cu proved difficult to fabricate because a critical heat treatment was necessary to obtain sufficient ductility. Besides, its rupture strength was shown to be low at operating temperatures, its electrical conductivity lower than desired, and its cost high. Furthermore, it often contained hidden flaws. The Nippert Electric Products Co. set out to find a better material by undertaking a research project with the stated objective of providing a material suitable for commutators that would have 1) a softening temperature above 750°F (400°C), 2) a minimum electrical conductivity of 90 pct of that of pure copper, 3) a strength not less that that of cold-worked silver-bearing copper, and 4) a materials cost of not over 1.5 times the cost of copper containing 25 to 30 oz Ag per ton. No commercial alloy met these specifications. However, it was found that copper containing from 0.18 to 0.35 pct Zr could be produced quite easily in the laboratory, and promised to fulfill the major requirements noted above. Interest naturally centered in the lower part of this composition range, since such alloys gave somewhat better electrical conductivities, and were lower in

Jan 1, 1958

By B. R. Hollebone

The chemical action of molten anhydrous pyridinium chloride (pyridine hydrochloride) on oxy salts and ores of some Group IV and V metals are discussed-in particular zirconium, hafnium, niobium (columbium) , and tantalum. Laboratory-scale experiments are described whose results suggest that this reaction might provide a practicable means of converting ores of these metals to the anhydrous metal chlorides. Experimental results are given which provide some insight into the nature of the reactions and some of the compounds which could be present at intermediate stages. The treatment of ores of the more refractory metals is difficult and expensive and often demands the use of gaseous chlorine, hydrogen fluoride, or other reagents which are, if nothing else, expensive and dangerous to use. This situation is, of course, due to the strong metal-oxygen affinity resulting from the high charge and the small size of the metal ion which combine to produce such high lattice energy in the metal oxide as to defeat standard reduction methods. Thus, the characteristic of these metals which leads to one of their most important properties—corrosion resistance—is the main hurdle in obtaining the metal. Many common methods' for treating ores of zirconium and niobium (columbium), for example, proceed as directly as possible to the preparation of anhydrous halides. These halides are purified by now standard processes of solvent extraction, fractional distillation, and so on. This paper reports on preliminary stages in the development of a method of treating these ores—particularly of niobium—so as to prepare the anhydrous, volatile halides by the use of chemical reagents which are much more easily handled than those used at present. CHEMICAL PRINCIPLES The solvent action of aminium halides has been referred to periodically in the literature over several decades. The chemistry of pyridinium chloride has been discussed particularly by Audreith2 and Starke.3 However, since this is not familiar chemistry in its nonaqueous setting, it is perhaps well to point out some general metallurgical principles and applications. One can use, as point of departure, the fact that HC1 dissolved in pyridine is an acid very much the same as aqueous HC1. It thus gives essentially all the reactions of the HC1 with which we are familiar. However, when the ratio of HC1:pyridine reaches 1:l (a ratio far higher than is possible with H2O) the solution becomes solid C5F5NHC1, pyridinium chloride.* Inter- estingly, the acidic properties of HC1 persist in this medium, although they are manifest only in the molten state of the compound. Some typical reactions of divalent metal compounds which we have carried out in our laboratories are the following: 2PyHCl + Zn — (ZnCl2) + H2 + 2Py 2PyHCl + MnO — (MnCl2) + H2O + 2Py 2PyHCl + CuS — (CuCl2) + H2S + 2Py 2PyHCl + CaCO3 — (CaCl2) + H2O + CO2 + 2Py In these equations, the parentheses indicate a solvated compound which in water would be predominantly a hydra ted cation but which in molten PyHCl will more likely be a complex chloro-anion of the type MC14-. Some important physical properties of pyridinium chloride (PyHCl) are given in Table I. One sees from the data in Table I that at the temperature of molten pyridinium chloride both water and pyridine will boil away. Thus the system will be kept anhydrous. For this reason the reaction 2NbCl5 + 5H2O— Nb2O5 + 10HC1 has no counterpart in molten PyHCl. Instead, the chloride is made even more stable by the formation of a hexachloro complex: Nb2O5 + 12PyHC1 — 2PyHNbC16 + 5H2O + 10Py One interesting property of these complexes is their thermal instability which for the case of niobium can be illustrated as PyHNbCl6 — PyHCl + NbCl5 With a view to possible use of this chemistry in ore treatment, we have attempted to dissolve Pyrochlore (essentially FeO - Nb2O5) and recover the NbC15 from it.

Jan 1, 1968

By P. Somasundaran, D. W. Fuerstenau

The length of the collector is found to influence the flotation of the mineral even at incipient conditions, which are below the concentration at which interaction at the solid-liquid interface begins to take place to form hemi-micelles. To study this dependence, concentration for incipient flotation of quartz was determined as a function of pH with collectors of various chain lengths. The observed effect of chain length on flotation is ascribed to that of collector adsorbed on the bubble surface. In previous studies, it was shown that at low concentrations the alkyl collector ions adsorb at the solid-liquid interface as individuals.''2 At higher concentrations, the collector ions adsorbed at the solid-liquid interface associate with each other to form two-dimensional aggregates called hemi-micelles. Above the hemi-micelle concentration, the length of the hydrocarbon chain is extremely important since the hydrocarbons are in effect removed from water during the association, making the energetic conditions more favorable for adsorption at the interface. Because of this enhanced adsorption, one observes a very rapid increase in flotation associated with the hemi-micelle formation at the solid-liquid interface. However, a dependence of flotation on the chain length at concentrations below that required for hemi-micelle association was also observed,' and this cannot be explained by the above mechanism which postulated hydrocarbon chain interactions only at the solid-liquid interface. This prompted an investigation into other possible reactions of the hydrocarbon chains and an examination of the conditions at the bubble surface involved in the flotation system and how these observations might explain the reactions at the solid-gas interface which cause the particle-bubble attachment required for flotation. To obtain more information on chain length effects, flotation, under incipient conditions, was tested by vacuum flotation techniques. The collector-concen-tration-pH relationships for flotation of quartz with alkyl ammonium acetate collectors was delineated by observing the pH at which quartz particles begin to float to the liquid surface. By investigating flotation as a function of pH, it was also possible to study the effect of neutral molecules on incipient flotation conditions, since the aminium ions hydrolyze to amine molecules at higher pH values. EXPERIMENTAL WORK Brazilian quartz specimens were crushed and sized, and the 270 x 400 mesh fraction was used for flotation studies. The samples were leached with concentrated hydrochloric acid until no coloration of the acid occurred. The leached material was washed free of chloride ions and stored in distilled water. The vacuum flotation technique developed by Schuhmann and prakash3 was used to determine the critical pH-concentration curves. This method, which can be used to delineate conditions for incipient flotation, is fairly simple and rapid. About 0.5 gm of 270 x 400 mesh quartz was placed in a 100 ml graduated cylinder which was then filled to the 100 ml mark with the collector solution made from high-purity alkyl ammonium acetate salts. The water used for the test was conductivity water saturated with air that had been passed through a cleansing train consisting of Drierite, Ascarite, a water wash bottle, and a trap. After the pH was adjusted, the cylinder was then conditioned for thirty minutes. In the tests where an acid pH was desired, sufficient acid was added before the collector solution to avoid any effect due to slow desorption of collector from the quartz surface. After conditioning, vacuum was applied to the system and the flotation or nonflotation of the quartz was noted. The pH at which the quartz particles began to float to the liquid-gas interface was taken as the critical PH. Critical pH curves were thus determined for different concentrations of the various collectors. Hallimond tube flotation data were taken from the authors' previous publication1 for correlation with that from the vacuum flotation. RESULTS AND DISCUSSION The results of vacuum flotation studies for determining critical pH-concentration curves, i.e., curves which delineate conditions for incipient flotation, are shown in Fig. I. In generaI, all the curves exhibit an upper and lower pH limit between which flotation will

Jan 1, 1969

By B. C. Mariacher

EXTRACTION of uranium from ores is being ac-complished by processes which. for the most part, subject the entire ore to acid or carbonate leaching. Ore deposits with a U 3 O 8 content below 0.10 pct U 3 O 8 are seldom considered suitable for treatment by leaching. A preliminary concentration that would enrich the uranium content of an ore by a simple, low cost process based on physical properties of the ore might result in some low grade deposits becoming commercial ores. In addition, the process might be employed in existing operations to reduce transportation and leaching costs and to increase capacity of existing leaching plants. A study to attempt the development of a preliminary concentration process for primary uranium ores was undertaken by the Colorado School of Mines Research Foundation under sponsorship of the U.S. Atomic Energy Commission. The objective of this work was to produce concentrates containing 0.25 pct U3O8 from the low grade ores tested. Ores Tested: The main effort was devoted to the low grade primary uranium ores from northwestern Saskatchewan. Samples were obtained from the Beaverlodge operation of the Eldorado Mining & Refining Ltd. Additional primary ores, obtained from deposits in Gilpin County, Colo., contained from 0.07 to 0.10 pct U3O8. Summary of Concentration Tests: The Beaverlodge ore was tested to determine amenability of the ore to concentration by magnetic, electrostatic, gravity, and scrubbing processes. None of these produced satisfactory results. Both gravity and magnetic processes produced fairly good concentrates when closely sized fractions of the ore were treated, but on the basis of treating the total ore, recovery was poor. Preparation of sized fractions and the low capacity of equipment for suitable concentration made these methods impractical. As flotation offered the advantage of treating the total ore without intermediate sizing, the main effort was in this direction. A flotation process was developed that fulfilled the concentration objectives as set by the AEC. Pilot plant testing was used to verify results obtained from laboratory batch testing. Mineralogy: A petrographic examination of the Beaverlodge ore included a study of polished sur- faces and identification of the radioactive mineral by autoradiograph and X-ray diffraction. Approximate quantitative mineral identification was as follows: quartz, 60 pct; orthoclase feldspar, 20 pct; chlorite, 10 pct; carbonates, 5 pct; and miscellaneous minerals, 5 pct. Included in this last group were plagioclase feldspar, pyrite, mica, chalcopyrite, pyroxene, sericite, magnetite, galena, and uraninite. The most general occurrence of uraninite was in the form of crusts and thin coatings on limonite-stained grains of pyrite, quartz, and pyrite-quartz intergrowth. At least 90 pct of the uraninite was still attached to other minerals in a 100 by 200-mesh size fraction. The uraninite crusts were as small as 10 to 20 µ diam, and 5 to 10 µ thick. The Flotation Process Petrographic examinations of the Beaverlodge ore had indicated the impracticability of attempting to concentrate the uranium by floating individual grains of uraninite. Liberation of the uraninite required grinding to sizes below those suitable for flotation. However, there was preferential association of the uraninite with some minerals while others were free of uraninite attachment. The approach to the development of a flotation process was, therefore, based upon an attempt to concentrate the uraninite by floating carrier minerals. The following paragraphs discuss the various stages of the process with regard to the factors tested and the conditions under which best results were obtained. Grinding: The most effective size range for flotation was —150 mesh + 13 µ. The —13 µ material in the final concentrate had a higher U3O8 content than the total ore, but not as high as the average concentrate; however, rejection of slimes before flotation was prohibitive because of the loss in uranium carried in the —13 µ fraction. Grinding techniques which contributed to a minimum production of fines, such as stage grinding, were then employed. Quartz and Silicate Depression: These minerals represented approximately 80 pct of the ore and were free to a large degree of uraninite attachment. Significant improvement in the grade of the concentrate was obtained by depression of these minerals with hydrofluoric acid or sodium fluoride. Promoter: Selective stage flotation of uraninite carrier minerals was simplified by development of a single promoter mixture. The mixture consisted of an emulsion of a fatty acid, fuel oil, and a petroleum sulfonate and was selected after a comprehensive series of tests. It contained three parts by weight of an oleic and linoleic acid such as Emersol 300,

Jan 1, 1957

By Douglas J. Robinson

A pilot scale process has been developed to separate mercury, tin, silver, and copper from dental amalgam scrap. Laboratory research led to a process which was operated in 55 gallon drum sized reactors to treat 2000 Tr oz charges of scrap per day. This paper discusses the development work, presents a flowsheet and gives an indication of the equipment necessary to carry out the process on a commercial scale.

Jan 1, 1984

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

AISI constructional alloy steels are a series of steels in which a numbering system signifies the chemical composition limits. SAE (Society of Automotive Engineers) and AISI (American Iron and Steel Institute) use basically the same numbering system. The steels contain, in part, alloy additions of chromium, molybdenum, nickel, and vanadium. They are used widely in the automotive industry but have not been adopted for high temperature service. The purpose of this investigation was to study changes in microstructure observed in typical AISI constructional alloy steels in the welded and un-welded conditions after exposure for 34,000 hr at 900" and 1050" and, in several instances, 1200°F. The tensile and creep rupture properties after exposure for 10,000 hr were also evaluated. The investigation is a continuation of the work previously discussed. Little was known concerning the existence of graphite in medium or low carbon steels before 1943. It is important to note that continued exposure at elevated temperature is required in order to develop graphite in steels. Interest in the presence of graphite in steel, and also in changes in the properties of steels after long service at elevated temperatures, developed after 1943 when a failure of a welded joint of high temperature piping was associated with the graphitization of a relatively low carbon content steel with 0.50 pct Mo,8,0 Numerous investigations have beeen made in recent years studying the relationship of this type of failure to changes in properties. Attempts have been made to evaluate the performance of a number of steels, particularly in the heat-affected zone of welds. It was the unfortunate failure of a weld-heated zone in high temperature piping in the steam-power industry which focused attention upon possible failures, and upon the need for improved steels for high temperature piping service. Investigation by the National Tube Div., U. S. Steel Corp., Lorain Works, has included a wide variety of steels in an attempt to learn the effects of numerous factors and elements upon the long time performance of steels, although many of the compositions studied will never be used at elevated temperatures.1,4-7 Included were the well established AISI steel series, which offered opportunity to test moderately high carbon content steels as well as observe the effect of nickel, chromium, molybdenum, etc., upon the properties of these well known steels. The properties of the AISI steels were also studied for comparison with the previously reported properties of the Cr-Mo steels, now used by the steam-power industry.5,7 Materials and Testing Procedure The AISI alloy steels in Table I were exposed for 10,000 and 34,000 hr at 900°, 1050°, and 1200°F.

Jan 1, 1958

By T. P. Papazoglou, N. A. D. Parlee, W. C. Phelps

PRACTICAL designs for good "home made" molybdenum furnaces are hard to find in the literature. The one described briefly below left something to be desired but was good enough to operate as a rather long (30 in.) two-zone furnace for periods of over 2 months at temperature (1400° to 1600°C) without shutdown. The principal problem in our application was to establish a temperature profile with two distinct constant-temperature zones and no dip between the zones. This and other problems mentioned below would not arise, however, if both zones were operated at the same temperature and if a shorter furnace were acceptable. Since molybdenum windings oxidize very rapidly when heated in air, impervious refractory tubes were used for both the furnace core and the outer jacket tube shown in the accompanying figures. A protective atmosphere of forming gas (10 pct H2, 90 pct N2) was continuously passed through the gas-tight annular volume between the core and outer jacket. The water-cooled copper ends shown in Figs. 1 to 3 sealed the ends of the tubes. Annealed molybdenum wire (40 mil) was wound on the recrys-tallized alumina core (35.5 mm OD by 28.5 mm ID by 30 in.) at a spacing of 0.36 in. The spacing was reduced to 0.29 in. close to the ends to partially compensate for end heat losses. Fig. 2 shows two molybdenum-ground lead taps off the center of the winding to produce the two independect temperature zones. The ground lead was insulated with 1/4-in. alumina tubing and connected to the grounded copper end by passing the wires through the gas port tube and crimping each wire into notches cut at the mouth. To prevent sagging of the core at high temperatures, refractory "troughs" were cut from alumina and mullite tubing to cradle the core. The support "troughs" which were 6 in. long and located about 5 in. from each end of the annular volume also served as radiation shields. In view of the different expansion coefficients and operating temperatures of the core and outer jacket (3.5 in. OD by 3 in. ID by 30 in.), the ends of the tubes were smoothed and squared to produce good sealing surfaces, and the core was ground 1/32 in. shorter than the outer tube. The power terminals were passed through their respective conductor ports which were internally lined with alumina tubing and sealed with Armstrong adhesive A-6 leaving about 1 in. of protruding lead wire for external connections. (Adhesive A-6 is a two-component system consisting of an epoxy-type resin with a mineral fibrous filler and an amine catalyst.) Figs. 1 and 3 show the entire assembly of concentric refractory tubes, copper ends, and sealing o rings, held together with two brass flanges and 3/8-in. bolts with heavy springs for dimensional flexibility. The furnace shell (19 by 19 by 30 in.) consisted of a steel frame with sheets of transite forming a box. The copper ends protruded through two 3.75-in. circular holes cut at the center of each transite square end. Thermal insulation next to the transite exterior was effected by K-23 B&W bricks alld in a central volume of approximately 9 by 9 by 30 in. a row of K-30 bricks was lined up to support the hot assembly. The rest of the volume around the outer

Jan 1, 1965

By P. G. Nahin, A. Grenall, R. S. Crog, W. C. Merrill

A progress report of an experimental investigation into the role of clay in reservoir performance is presented. The Paper gives some of the reasons for considering clay as a significant component and outlines the objectives of a broad field of stud) which it is intended to pursue. Descriptions of the analytical methods used are given; these include X-ray diffraction. elec tron miscroscopy, thin section petrography, infrared spec-troscopy, and cation exchange analysis. A suite of the more important clay minerals has been assembled and characterized l~y these methods for use as standards in core analysis. From the data obtained it appears that although no one method of analysis is diagnostic for all of the clay minerals the infrared technique shows considerable promise in this direction. For the present, one or more supplementary methods should be used to confirm the clay mineral identifications. The methods of analysis are applied to field cores taken from repesentative and widely differing strata especially as regards their susceptibility to damage by fresh water. well.; completed in the stevens and Gatchell zones in San Joaquin valley are I,articularly clear-cut examples of this behavior with stevens zone wells being more adversely affected by fresh water. cores from these zones have been studied and are discussed. It appears that differences in this behavior can be ascribed to differences in the nature of the contained clays. The value of the infrarecl spectra of the clay fractions in establishing the identity of the predominant clay minerals is given particular emphasis. INTRODUCTION It is a challenge to the technical resources of the petroleum industry that when the economic limit of production is reached, from 40 to 70 per cent of the oil in California reservoirs remains unproduced even by use of the best presently known methods of recovery. The magnitude of this abandoned volume of oil can be appreciated when it is considered that to 1950 in excess of 8 billion bbll has been produced from California reservoirs with estimated economically recoverable reserves in known fields and pools totaling nearly 4 billion bbl.24 If for every barrel of oil produced there is at least another barrel still in place, it is evident that the revenue obtained from the recovery of only a .few per cent of this volume would repay the cost of the required research manyfold. From well completion experience. production behavior, and a growing body of laboratory data it now appears certain that the mineral composition of a producing stratum has an important bearing on the productivity and ultimate yield. In addition to the organic component and water, the cores con,ist of gravel, sand. silt, and clay" in diverse variety of (a, composition and (b) texture. It is the composite effect of these two factors which is probably responsible in large measure for the way in which the oil flows to the well. The role of the clay and fine-size accessory minerals is not clear but there is a growing opinion, based on their physical and chemical properties, that it is a significant one. of particular importance are the prime facts: 1. The silt and clay fractions of the reservoir matrix possess the highest surface area per gram, and 2. The silt and especially the clay fractions are the most chemically reactive of the inorganic constituents present. Only within the last few years has the knowledge of clay mineralogy and the techniques of identifying the clay minerals reached such a stage as to enable reliable inquiry into the composition of argillaceous sediments.2,8,10,11,12,16,26 It is the purpox of this and succeeding papers to add to the fund of information on the role which these materials play in the production of petroleum from California formations by correlating their presence and associated properties with observed reservoir behavior. In the present paper attention is directed to their possible influence on damage by fresh water. OBJECTIVES The attack on this problem divides naturally into two broad phases: 1. Determination of the nature of the clays and their relationships to the other mineral components, and 2. Determination of the physico-chemical relationships between the clays and the interstitial fluids. In the work described in this paper the emphasis has been on phase 1, which stems logically from the necessity of identifying and understanding the materials to be dealt with in Phase 2. Based on the authors' present opinion that not all of the minerals which occur in oil-bearing formation are of equal importance in their effects on the flow and recovery of oil, it was decided to focus attention first upon the clay minerals content and then. later perhaps. work into the field of the normally larger size non-clay minerals and fractions. The

Jan 1, 1951

By W. C. Merrill, P. G. Nahin, A. Grenall, R. S. Crog

A progress report of an experimental investigation into the role of clay in reservoir performance is presented. The Paper gives some of the reasons for considering clay as a significant component and outlines the objectives of a broad field of stud) which it is intended to pursue. Descriptions of the analytical methods used are given; these include X-ray diffraction. elec tron miscroscopy, thin section petrography, infrared spec-troscopy, and cation exchange analysis. A suite of the more important clay minerals has been assembled and characterized l~y these methods for use as standards in core analysis. From the data obtained it appears that although no one method of analysis is diagnostic for all of the clay minerals the infrared technique shows considerable promise in this direction. For the present, one or more supplementary methods should be used to confirm the clay mineral identifications. The methods of analysis are applied to field cores taken from repesentative and widely differing strata especially as regards their susceptibility to damage by fresh water. well.; completed in the stevens and Gatchell zones in San Joaquin valley are I,articularly clear-cut examples of this behavior with stevens zone wells being more adversely affected by fresh water. cores from these zones have been studied and are discussed. It appears that differences in this behavior can be ascribed to differences in the nature of the contained clays. The value of the infrarecl spectra of the clay fractions in establishing the identity of the predominant clay minerals is given particular emphasis. INTRODUCTION It is a challenge to the technical resources of the petroleum industry that when the economic limit of production is reached, from 40 to 70 per cent of the oil in California reservoirs remains unproduced even by use of the best presently known methods of recovery. The magnitude of this abandoned volume of oil can be appreciated when it is considered that to 1950 in excess of 8 billion bbll has been produced from California reservoirs with estimated economically recoverable reserves in known fields and pools totaling nearly 4 billion bbl.24 If for every barrel of oil produced there is at least another barrel still in place, it is evident that the revenue obtained from the recovery of only a .few per cent of this volume would repay the cost of the required research manyfold. From well completion experience. production behavior, and a growing body of laboratory data it now appears certain that the mineral composition of a producing stratum has an important bearing on the productivity and ultimate yield. In addition to the organic component and water, the cores con,ist of gravel, sand. silt, and clay" in diverse variety of (a, composition and (b) texture. It is the composite effect of these two factors which is probably responsible in large measure for the way in which the oil flows to the well. The role of the clay and fine-size accessory minerals is not clear but there is a growing opinion, based on their physical and chemical properties, that it is a significant one. of particular importance are the prime facts: 1. The silt and clay fractions of the reservoir matrix possess the highest surface area per gram, and 2. The silt and especially the clay fractions are the most chemically reactive of the inorganic constituents present. Only within the last few years has the knowledge of clay mineralogy and the techniques of identifying the clay minerals reached such a stage as to enable reliable inquiry into the composition of argillaceous sediments.2,8,10,11,12,16,26 It is the purpox of this and succeeding papers to add to the fund of information on the role which these materials play in the production of petroleum from California formations by correlating their presence and associated properties with observed reservoir behavior. In the present paper attention is directed to their possible influence on damage by fresh water. OBJECTIVES The attack on this problem divides naturally into two broad phases: 1. Determination of the nature of the clays and their relationships to the other mineral components, and 2. Determination of the physico-chemical relationships between the clays and the interstitial fluids. In the work described in this paper the emphasis has been on phase 1, which stems logically from the necessity of identifying and understanding the materials to be dealt with in Phase 2. Based on the authors' present opinion that not all of the minerals which occur in oil-bearing formation are of equal importance in their effects on the flow and recovery of oil, it was decided to focus attention first upon the clay minerals content and then. later perhaps. work into the field of the normally larger size non-clay minerals and fractions. The

Jan 1, 1951

By HILLARY W.

THAT colleges and technical schools constitute a vital factor in our industrial system is being realized more and more of late years. Consequently it is desirable that there should be a constant interchange of ideas between the 'school and the industries and that there should be a more intimate contact between the student and his future employer. Business and industry demand certain proficiencies and qualifications of the student and he, in turn, sees certain rewards and advantages in the industry. . In a meeting of this kind, whose primary purpose is to promote a greater intimacy between the students and those men who are active in the mining profession, it is quite fitting that each state his demnds upon the other in order to establish a common understanding. It is probable that a student, not being conversant with actual conditions in the industry, may be unfair in what he asks of his employer. Therefore criticism, constructive or other- wise, is not only accepted, but is invited.

Jan 1, 1930

department, first as a practical miner, next. as rodman on the survey corps, of which he soon became chief, then draftsman and mining engineer in the company's office. In January, 1916, he was promoted to the position of district engineer in charge of mining engineering work. He became a member of this Institute in September, 1917. Captain Ba.llamy's military experience began at the same time as his engineering practice. He was a charter member of Company A, Engineers, N. G. P., which was organized ten years ago. He saw service on the Mexican border as First Lieutenant of this Company, and remained in that position until November, 1916. In July, 1917, he was again called into service and was sent to Camp Hancock, Ga., with the 103d Regiment of Engineers. Before joining this regiment he attended a school for officers at Fort Sill, Okla., where he received special training in field fortifications. In December, 1917, he was commissioned Topographical Captain on the Regimental Staff, and in April, 1918, preceded his regiment by about six weeks to France, where he again attended an officers' training school. He rejoined his regiment on July 15, near Chateau Thierry and was killed near Fismes on Aug. 9, 1918. Lieutenant Martin F. Bowles Martin F. BOWleS, born Apr. 25, 1893, at Bonne Terre, Mo., and graduated from the Neodesha, Kans., High School, had finished all but one month of a four-year course in metallurgical engineering at the Missouri School of Mines, Rolla, Mo., when on May 12, 1917, he entered the first Officers' Training Camp at Fort Riley, Kans. At the close of the training period, he was commissioned a Sccond Lieutenant and assigned to Co. B, 355th Infantry, 89th Division, and stationed at Camp Funston. He left this camp with his company on May 21, 1918, and sailed from an eastern port on June 4, ayriving in England on June 15, 1918. After a short stay at a rest camp there, he proceeded to France. On August 14, he wrote that he was with Battalion Headquarters as Gout Officer, 1st Battalion, 355th Infantry, 89th Division. The last letter received from him, dated September 2, was written in his dugout and contained the following: "Here it is 2.45 a. M. Sitting in a dugout waiting for some patrols to report back in, I am writing this by the light of two candles." He was killed in action on the night of Sept. 3, 1918. The letter of notifi-

Jan 1, 1920

By Gen-ichi Nakazawa, Masamichi Fujimori, Ichiro Doi

INTRODUCTION The major products of nickel industry in Japan are the electrolytic nickel (E-Ni), the ferro-nickel (Fe-Ni) and the nickel oxide sinter (NOS), totaling in production to 90 - 100 X 103 tons/year in terms of pure nickel content, and sharing approximately 20% for E-Ni, 10% or less for NOS, and the rest for Fe-Ni. The raw materials to be used for these products depend totally upon the imports from abroad; matte, the raw material used in the production of E-Ni, is from Australia and Indonesia; matte for the NOS is from Indonesia and New Caledonia; and garnierite, the raw material for Fe-Ni, is imported in bulk from New Caledonia, Indonesia and the Philippines. This report describes the acquisition of these raw materials, the production processes, trend of supply-demand, problem areas and the measures taken, and so forth, in connection with the nickel industry in Japan. ELECTROLYTIC NICKEL 1. History The nickel industry in Japan began in 1939 by the Sumitomo Metal Mining Co., Ltd. (SMM) with 150 tons E-Ni/month under the blast furnace smelting and the metal anode electrolysis. This was temporarily suspended after the end of last World War II, but resumed in 1952 with garnierite of New Caledonia as a raw material. Since then, the production capacity has been expanded incidentally to the increase of demand. However, since the smelting of garnierite contained about 2% nickel was very costly, the smelting process had been changed to smelt the briquettes of the mixture of garnierite and nickel sulfide concentrate imported from Canada and Australia. In 1975, this smelter was closed, and SMM's nickel refinery used matte from Western Mining Corp. (WMC) of Australia as a raw material. The refining process had been the metal anode one. The crude nickel oxide derived from roasting the high grade nickel matte had been melted and reduced with coke in the electric furnace and cast into anode. In 1970, a new refinery was constructed to produce 1,000 tons Ni/month under the matte anode process, and further, in 1976, the old refinery was converted into the matte anode process, thus resulting in the total production capacity of 1,690 tons Ni/ month today under the matte anode process. Shimura Kako Co., Ltd. began in 1951 to produce a little of E-Ni, and in 1955, they constructed a shaft furnace smelter with New Caledonian garnierite as a raw material to begin the E-Ni production under the matte anode process. Its monthly production reached 400 tons in 1957, but it discontinued its smeltering in 1963 to convert to the matte import from S. Le Nickel, WMC and INCO. In 1979, it changed the source of matte supply from the above to Soroako of Indonesia, discontinued the E-Ni production in 1979, and arranged for a total toll contract with Sumitomo. Meanwhile, SMM has developed a very distingished process for nickel-cobalt separation and refining by a solvent extraction method from nickel and cobalt mixed sulfide generated as a by-product in the nickel recovering process from laterite under the Nicaro process. Nippon Mining Co., Ltd. (NMC) also developed its own process. The plants under these processes were constructed in 1975, with the monthly production capacity of 230 tons of nickel and 130 tons of cobalt by SMM, and 300 tons of nickel and 110 tons of cobalt by NMC. SMM imports the raw material from the Marinduque Mining and Industrial Corp. of the Philippines, while NMC from Queensland Nickel Pty. Ltd. of Australia. 2. Production Status 2.1 Producers and materials Today, SMM holds the monthly E-Ni production capacity of 1,920 tons, of which 1,690 tons are from the matte anode process, and the remaining 230 tons are from the mixed sulfide as a raw material. NMC also uses the mixed sulfide as a raw material for a production of 300 tons/month. [ ] Most of SMM's raw material, nickel matte, is imported from WMC of Australia, partly using the Soroako matte from Indonesia. An example of material analysis is given in Table 1. Matte is a raw material for E-Ni and NOS, and the major sources of matte supply at present are Australian WMC and Indonesian Soroako, occupying ap-

Jan 1, 1982

Boiler-Room Economy "Establishing and Maintaining Boiler-room Economy" is the title of a paper presented before the Ohio Society of Mechanical Electrical and Steam Engineers by Geo. H. Gibson, of which the following is an excerpt: Boiler-room economy depends less upon equipment than upon operation, i.e., it depends largely upon the condition in which the apparatus is maintained and how it is used. A given boiler may operate this week with an efficiency of 78 per cent., and next week with an efficiency of 65 per cent., while using the same fuel and developing the same rating. If there are variations ii; character of fuel and in load and other factors, the falling-off may be even greater, possibly to less than 60 per cent. The steam produced may cost twice as much per 1,000 lb. at one time as at another. Most steam plant managers know from their own experience that these statements are not exaggerated. It does not take much of a plant to run up a coal bill of $5,000 per year, many "spend $10,000 for coal, and fuel bills of $50,000, $100,000, or $200,000 per annum are not uncommon. As it call be shown in the majority of these plants that 10 per cent. of this amount may be saved, and in large numbers of them 25 per cent., while in some the expenditure can be cut in half, there is no disputing that we have here a subject worthy of attention. In the production of steam the greatest variable is the human factor. Before we can pass judgment, however, we must first have standards. This implies accurate quantitative knowledge of fuel consumption and steam production. We must measure the output and know how much the steam costs per thousand pounds, and how many pounds of steam are obtained from a pound of coal. We can then begin to analyze the problem, and find where and how methods and conditions can be improved, and how much. Many favor buying coal on a B. t. u. basis. This is advisable where the amount purchased warrants the considerable expense involved in systematically gathering samples that: are. truly representative and in having analyses made, of every carload. Coal analyses, combined with. an honest endeavor on the part of the miner to ship good coal, should insure the receipt of the heat units paid for. , It often happens, however, that the coal which is cheapest on a B.t.u. basis is not the cheapest or most suitable for producing steam, because of peculiarities of the plant in which it is to be burned, or conversely, the fuel which furnishes cheap B.t.u. may require special methods or equipment for its economic utilization.

Jan 2, 1916

By C. Richard Honeycutt, Frederick C. Langenberg, Guenter Pestel

Otto Schaaber (Institut für Harterei-Technik, Bremen-Schönebeck, Germany)— Langenberg, Pestel, and Honeycutt gave an interesting example of the grain refining effect nonstationary magnetic fields may execute on a solidifying metal. Probably some additional comments, based on more than a decade of experience with this method of influencing crystallization, may be useful. They refer to an attempt to explain the mechanism of grain refinement by such fields, and to recent European developments which have not been mentioned in the paper. I. During studies of the temperature distribution in a metal body near the phase boundary solid/liquid, an anomaly was observed under certain special conditions: a) direction of heat transfer as horizontal as possible, b) steady state (equilibrium, i.e,, solidification resp. melting rate exactly zero). In the liquid phase, immediately adjacent to the phase boundary, the temperature was found to be constant over an appreciable distance in spite of a high value of heat transfer (40.000 to 70.000 keal/ m2h).3 Convection, which might explain this phenomenon, could not be observed. Therefore another explanation had to be sought. The assumption that a metallic melt, especially at temperatures near the point of solidification, contains some sort of atomic arrangement with a higher degree of order than the surrounding liquid, now is generally accepted. Considering the differences in energy between such an arrangement and its environs, a transport of heat even in absence of any temperature gradient is conceivable by continued formation and redissolution of regions with a higher degree of order, i.e., with lower energy level.3 At this stage, it was not necessary to postulate any special condition as to the form or size of these regions or the distance between arrangements to be newly formed and those to be redissolved. However, a simple consideration shows that an energy transfer from one region to another will only be possible without loss of energy, if the distance between will be equal to the lattice parameters, and if, secondly, crystallographic axis or planes will be parallel.4 By the way, this assumption might give a reasonable explanation of the well known orientation effect of the heat flow during solidification. Any measures to prevent columnar crystallization should act upon this ordering mechanism: a) the regions with a lower energy (higher order) should not be allowed to arrange themselves parallel to the direction of heat flow, and their growth should be disturbed; b) all conditions leading to an appreciable heat flow of uniform direction should be avoided or removed. Condition a) may be satisfied by a physical force preferably under 90 deg to the main axis of the columnar crystals (i.e., parallel to the solidification front) acting on the ordered regions; condition b) by equalizing any differences in

Jan 1, 1962

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

The solid solubility of iron in 2 to 10 pct cupro-nickels increases with temperature and nickel content. Property changes accompanying various heat treatments indicate typical precipitation hardening behavior. Iron content also affects softening temperature and sub-scale formation. These factors, as well as impingement corrosion resistance, influence the optimum iron content of commercial alloys. FOR many years Cu-Ni alloys have been used extensively in the form of tubes, pipes, and plates for the construction of salt-water lines and surface condensers on shipboard and in tidewater power stations. The 30 pct Ni alloy has been considered more resistant to rapidly flowing sea water than alloys of lower nickel content, and has been standard on ships of the U. S. Navy. Some ten years ago, the still better corrosion resistance obtained by modifying the 30 pct Ni alloy with approximately 0.5 pct Fe was recognized, and the iron-bearing alloy rapidly superseded the plain alloy as the standard material for severe service. In 1945, Tracy and Hungerford1 published a study of the effect of iron on the corrosion of various cupro-nickels in sea-salt solutions, and their data indicated that the 10 pct Ni alloy containing about 0.75 pct Fe was equivalent to the 30 pct Ni alloy containing 0.5 pct Fe. This was confirmed by LaQue in discussion of the above paper, and by results in an experimental condenser set up at the Kure Beach marine test station of The International Nickel Co., reported by Freeman and Tracy.' The 10 pct Ni iron-bearing alloy is now being very widely used in applications where the 30 pct Ni iron-bearing alloy was formerly considered standard. While this "substitution" has undoubtedly been stimulated by the present extreme shortage of nickel, it must be emphasized that it involves no loss of service performance, and would have occurred anyway in the course of time, for economic reasons. In view of the increasing use of the 10 pct alloy, it seems desirable to make generally available the results of several investigations of Cu-Ni-Fe alloys carried out in the Metallurgical Research Laboratory of The American Brass Co. in recent years. The present paper, deals with the constitution of these alloys in the copper-rich corner of the system, and with the variations in hardness and tensile properties resulting from the heat treatment of alloys containing various amounts of iron. Most of this work is concerned with alloys containing 10 pct Ni. With over about 0.75 pct fe, the 10 pct Ni alloy is suscep- Alloys Several series of cupro-nickel alloys containing iron were used in these investigations. Most of them were prepared in the laboratory, but two samples of commercially fabricated alloys were included. Series A—Nominally 2 and 5 pct Ni, each with 0 to 1.5 pct Fe. Series B—Nominally 10 pct Ni with 0.1 to 0.4 pct Fe. Series C—Nominally 1.0 pct Ni with 0 to 2 pct Fe. Series D—Nominally 10 pct Ni with 3 to 5 pct Fe. Series E—Nominally 10 pct Ni with 1 and 1.5 pct Fe.

Jan 1, 1953