Search Documents

By S. R. Zimmerley, S. F. Ravitz

High-grade cobalt concentrates were produced from the complex Blackbird ore with very good recovery in continuous pilot-plant operations in which a low-grade bulk cobaltite-pyrite flotation concentrate was roasted in a multiple-hearth furnace to oxidize the pyrite selectively. The cobaltite was floated from the resulting calcine. THE existence of the cobalt-copper deposits in the Blackbird district, Lemhi County, Idaho, has been known for many years. However, these deposits have not yet been exploited successfully because of the low grade of the ore, absence of information on ore reserves, and lack of feasible methods for concentrating and recovering cobalt from the ore. In 1941, when it appeared that World War II might interfere seriously with imports of cobalt from overseas, the U. S. Bureau of Mines started an extensive mining and metallurgical investigation of the Blackbird deposits. Exploration by trenching and drilling1 indicated that ore reserves were adequate to warrant consideration of large-scale exploitation. A process for producing high-grade cobalt concentrates from the ore was developed at the Salt Lake City Station of the Bureau,2 and hydrometallurgical procedures for producing cobalt metal or oxide from the concentrates were developed at the Boulder City Station.3 The Howe Sound Co., through a subsidiary, the Calera Mining Co., carried out further exploratory work, which increased probable ore reserves to a tonnage commensurate with a large investment in mine, mill, transportation facilities, and refinery. Simultaneously, the metallurgical staff of the company, working in cooperation with the Bureau of Mines, further investigated the metallurgical problems. It was the opinion of both groups that pilot-plant testing was required to translate laboratory results into plant operation. In general, the Blackbird ore has a high content of pyrite and some pyrrhotite and contains 0.5 to 1 pet cobalt and 1 to 2 pet copper, which are present essentially as cobaltite and chalcopyrite. The copper can be recovered readily as a high-grade concentrate by selective notation. The cobalt then can be recovered as a bulk sulphide concentrate assaying 4 to 5 pct cobalt, but no satisfactory procedure for separating the cobalt from the pyrite and pyrrhotite directly by flotation had been found. The method developed by the Bureau for producing a high-grade cobalt concentrate is essentially an application of the old Horwood process of selective roasting.4 The bulk sulphide concentrate is roasted to form an oxide coating on the iron mineral particles, and the calcine is then treated by flotation. The oxide coating prevents the iron minerals from floating so that it is possible to obtain a high recovery of cobalt in concentrates assaying more than 20 pct cobalt. Laboratory tests by metallurgists of both the Bureau and the Howe Sound Co. had indicated the optimum roasting temperature to be 425° to 450°C. At lower temperatures the rate of oxidation of the iron minerals is too low, whereas at higher temperatures substantial quantities of cobalt are rendered water-soluble. Because of its high sulphur content (35 to 40 pct), the bulk concentrate tends to continue to burn after it has reached the optimum roasting temperature. Although excessive temperatures could be avoided in the small-scale laboratory furnaces, there was considerable doubt that the temperature could be controlled properly in industrial equipment. To provide material for the pilot-plant tests, the Calera Mining Co. installed a small, temporary flotation mill at the Blackbird property and treated

Jan 1, 1951

By Phillip E. La Moreaux

Fluoride, generally less than 0.5 ppm, is present in ground water from rocks of Paleozoic age and older, in northern and eastern Alabama. Some of the water-bearing formations in the Coastal Plain area of the State yield water with as much as 6.8 ppm fluoride. IN June 1940, the U. S. Geological Survey, in cooperation with the Geological Survey of Alabama, began a study of the ground-water resources of the part of Alabama where water is obtained from Cretaceous rocks. The purpose of the study was to determine the quality, quantity, occurrence, and availability of ground water in that area. These studies have been expanded to include ground-water investigations in the area of Tertiary rocks, or southern quarter of the State, and certain areas in northern Alabama. The first report issued on these studies was by C. W. Carlston,1 of the Alabama Geological Survey. In the present paper all references to ground-water data for the Cretaceous area are taken from this earlier publication. In 1945, the Dentistry Division of the Alabama Department of Public Health became interested in the correlation of tooth decay and mottled enamel with the chemical quality of ground water used for public supplies in the State. Through a cooperative arrangement between the State Department of Public Health and the Ground Water Division (now Branch) of the U. S. Geological Survey, a report by the author2 was published in 1948. These two reports give accurate information on the occurrence of fluoride in the Coastal Plain of Alabama. At present, only scattered information is available on fluoride in ground water of the crystalline-rock or Piedmont area and for the Paleozoic area of Alabama, but it is hoped that in the future more complete information on the presence of fluoride in ground water in these areas can be collected. Outline of Geology and Ground Water: As described by Adams,3 the State of Alabama includes parts of two major geologic divisions, the Appalachian region and the Coastal Plain. The boundary between these divisions is irregular and is known as the Fall Line of the Atlantic and Gulf Coast States. The Fall Line enters Alabama near Phoenix City, extends westward to Wetumpka, Clanton, and Tuscaloosa, and then swings northwestward to the northwest corner of the State. The Appalachian region in Alabama includes three major provinces, the Piedmont province, the Appalachian Ridge and Valley province, and the Appalachian Plateau province (fig. 1). The rock formations in the Piedmont province in east-central Alabama are mainly of pre-Cambrian age, chiefly crystalline schists and gneisses injected by younger igneous rocks (fig. 1, I). They are faulted and folded and have a complicated structure. These rocks are the oldest and among the most complex rocks in the State. Generally, only small yields of ground water are obtained from rocks in this area. Even though ground water is of great importance for the development of domestic and farm supplies in rural areas and a few small industrial and municipal wells, yields in the area from individual wells generally range from 5 to 25 gpm and rarely exceed 50 gpm. The geologic formations of the Appalachian Ridge and Valley province and the Appalachian Plateau province (see fig. 1, II, and III) are separated on the basis of their structure. These rocks are of Paleozoic age, ranging from Cambrian to Carboniferous, and comprise a succession of formations consisting chiefly of shale, sandstone, limestone, and dolomite, aggregating many thousands of feet in

Jan 1, 1951

INTRODUCTION Besides the European export credit agencies covered in Ted Rides' paper in this Chapter, other agencies are also active (see Appendix) but the most notable for mining projects are The Export-Import Bank of the United States ("US Exim") and the Export Development Corporation ("EDC") of Canada. Mexico's Fomex is basically a short-term trade-finance fund administered by the Central Bank. US Exim This independent agency can provide loans, guarantees, and insurance. Like all export-credit agencies, its mandate is to support the export of goods and services from the US as a means of competing against other countries' products. If a piece of mining equipment can only he made in the US, the US Exim may very well not provide any financial assistance. (It is important not to place the order for any item for which export credit is sought because, once ordered, the situation is no longer competitive in US Exim's eyes.) Direct Credits and financial guarantees ("buyer credits") are commonly in amounts greater than 85 million and for terms longer than six years. An example here is the $48.5 million provided to PT International Nickel Indonesia (see Robert de Gavre's paper in Chapter 12). US Exim usually requires a 15% downpayment and, therefore, finances up to 857 of the goods; less if the US content is lower. The dollar funding can he US prime, London Interbank Offered Rate (LIBOR), or other sources. Exim can fund in either or both of the following ways: 1. Under a US bank Letter of Credit ("L/C") 2. Reimbursement to the buyer/borrower via a US bank account. US Exim will, without charge, issue a preliminary commitment. It will, however, need to approve the various credit agreements and prefers to tie other parallel financings into one loan agreement. US Exim's total commitments are large, up to $5R billion in aggregate under various programs. US Exim has been the world's leader in medium-to long-term minerals project financings/ co-financings but suffers from (i) aggressive foreign export-credit competition whereby other nations mix in soft-loans or aid programs ("mixed credits") to increase the percentage financed and lower the interest margin and (ii) an imbalance in its own cost of funds. A common US Exim package would be as follows: 15% Banks under US Exim guarantee, floating rate over prime or LIBOR. 35% US Exim funding, fixed rate 35% Pefco funding, fixed rate 857 Drawn down pro-rata under US bank L/C 15% Cash down payment (may have been financed within a project/corporate credit) 100% Repayment usually begins six months after planned start-up in equal semi-annual instalments, with the banks usually paid out first, Pefco next, and US Exim last. Medium-term credits ("supplier credits") are issued for US equipment exports for terms up to five years, again for 85% of the equipment costs although the exporter is expected to bear at least 10% out of that 857 for its own risk. The buyer is required to be a first-class credit such as some governments or highly credit-worthy companies. Otherwise a bank L/C would be required. (This may be wrapped into an overall project-finance package for a minerals development. The project-finance banks provide an L/C to US Exim instead of funding that portion themselves.) US Exim guarantees 100% of the political risk and either 85% or 95% of the commercial risk for

Jan 1, 1985

By J. D. Forrester, Erich Sarapuu, T. C. Cheasley

John G. Tripp-—The concept of converting fuel deposits in-situ to useful forms of energy and chemical raw materials has important possibilities as a means of stretching out our fuel resources. The authors have worked in this field for years and in fact are among the pioneers in developing in-situ techniques based on underground electrocarbonization. Their efforts have aroused great interest in this subject and their contributions will undoubtedly gain even more significance as time goes on. The 4 to 5 billion tons of petroleum are proved reserves, that is, they are completely defined and could be produced economically with present methods of recovery. Reserves of coal, tar sands, and oil shale shown in Table I are not equivalent to proved reserves as the term is used in the oil industry. Incidentally, the 4.3 billion tons of oil shown in the tabulation is equal to about 28 billion barrels of oil and, therefore, presumably does not include reserves of natural gas liquids estimated at about 5 billion barrels. The relative comparisons would be more complete if these liquids together with the reserves of natural gas were included in the tabulation. It is stated in the report that production costs of the order of 10c per million Btu's could be expected from a large industrial electrocarbonization installation. The authors state that the operation probably could be operated successfully and at a profit. I would like to express my view that for the operation to be profitable extremely favorable conditions would have to prevail. For example, the coal seam would have to be thick and close to the surface in order to minimize drilling costs; the deposit should be dry and so situated that there would be little, if any, inflow of ground water; and the seam would have to be relatively gas tight to avoid excessive gas leakage. Notwithstanding the tremendous strides that have already been made, it is my hope that the authors plan to continue their development work. Experiments on underground electrolinking and initial carbonization at Gorgas, Ala., indicate a need for improved control over the operation. Subsequent examination of the underground system at Gorgas has shown that the gasification zone did not always follow a direct path between the electrodes. Undoubtedly the control of the in-situ thermal processes can be improved by further development work. With respect to the electrocarbonization of oil shale it may be well to point out that the cost of mining oil shale is estimated to be 50c to 60c per ton. These are low mining costs as compared to coal. Thus it would appear that there is less economic incentive for applying in-situ thermal methods to oil shale than there is for applying these methods to coal. As is the case with in-situ methods for petroleum, the product from the shale having the most economic interest would be liquid oil rather than gas. The authors point out that for distances up to several hundred miles it is cheaper to transmit energy as electricity than it is to ship energy as coal. This is a very important point, and with coal shipping rates rising periodically, it could prove increasingly important in the future. I believe that the authors deserve great credit for their outstanding work on underground electrocarbonization. The knowledge resulting from their efforts is of great value to our fuels technology. James L. Elder—The experimental work conducted by the authors on the electrolinking-carbonization of carbonaceous materials in situ is of great interest. The method is of great importance in the development

Jan 1, 1955

WE the undersigned, being all persons of full age and citizens of the united States, and a majority residents of the State of New York, desiring to form a corporation pursuant to the provisions of the Membership Corporations Law for the purpose of incorporating, as provided in Section 5 of Article I. of said law, the existing unincorporated association known as American Institute of Mining Engineers, do hereby make, acknowledge and file this Certificate for that purpose, and do Certify as follows: I. That the American Institute of Mining Engineers is an unincorporated association organized and existing with the object of promoting the arts and sciences connected with the economic production of the useful minerab and metals and the welfare of those employed in these industries by means of meetings for social intercourse and the reading and discussion of professional papers, and to circulate by means of publications among its members and associates the information thus obtained. II. That the persons duly appointed or designated to manage the affairs of said association are designated by the rules thereof Members of its Council; that the undersigned are all members of said Council as the same was constituted on the 20th day of December, 1904. III. That on said last-mentioned date a regularly called meeting of said association was held at its office in the Borough of Manhattan, City of New Pork; that thirty days before such meeting notice of the intention to incorporate said association was given by mail to each member thereof whose residence or post-office address is known; that at said meeting the following resolutions were offered, seconded and duly adopted by the unanimous vote of all its members then present, to wit: "Resolved, That it is the sense of the members and associates of the American Institute of Mining Engineers in general meeting assembled that it is desirable and necessary for the well being of said association and its members and for the furtherance of the objects for which the same has been formed, that said association lncorporate under the Membership Corporations Law of the State of New york; "And Further Resolved, That the Members of the Council of this Association, or a majority thereof, be and they hereby are authorized, in accordance with the provisions of Section 5 of Article I. of the Membership Corporations Law, to incorporate this association for the same purposes for which it has been organized and conducted, in the manner provided in Article 11. of said law; "and Further Resolved, That the name of said corporation as hereby adopted by this meeting shall be American Institute of Mining Engineers; "And Further Resolved, That the said incorporators shall be named in the Certificate of Incorporation as directors of such corporation until its first annual meeting, and that such directors and their successors in office shall be and they hereby are authorized to enact and adopt a Constitution and By-Laws for the government of said corporation." IV. That the name of the proposed corporation is American Institute of Mining Engineers. V. That the purposes for which this corporation is to be formed arc: To promote the arts and sciences connected with the economic production of the useful minerals and metals, and the welfare of those employed in these industries by all lawful means; to hold meetings for social intercourse and the reading and discussion of professional papers, and to circulate by means of publications among its members the information thus obtained, and to establish and maintain a place for meeting of its members, and

Jan 1, 1929

By S. R. B. Cooke, W. Philippoff, Donald E. Cadwell

[THE importance of contact angles in flotation has long been recognized, but little has been done to get quantitative relationships between the surface coverage of the mineral by the reagent, the length of the hydrocarbon chain, and the contact angle. It is well known that for a complete monolayer on the surface of a mineral the contact angle ? is determined only by the reagent&apos; and principally by the chain length of the hydrocarbon radical. Although for flotation the monolayer usually is regarded as being complete, early experiments of Wark and Cox2 showed that at very small concentrations of potassium ethyl xanthate the contact angle on galena changed in a continuous way from 0° to the equilibrium value of 60°. Further, Gaudin and Vincent&apos; showed a similar continuity using heptylic acid and sphalerite. This shows that with probably incomplete monolayers, ? varies with the degree of surface coverage. At the time these experiments were made it was impossible to measure the actual amount of surface coverage, especially since the decrease of the collector concentration in the liquor could be influenced by chemical side reactions. Through the use of the radioactive tracer method for the measurement of the amount of collector adsorbed on the surface of the mineral, Gaudin and Bloecher4 were able to determine accurately the actual surface coverage of dodecylamine acetate on quartz, but they did not measure any contact angles. It is believed that the relationship between the surface coverage and the contact angle is extremely important in flotation, especially as Gaudin and Bloecher showed that a 95 pct recovery is possible with a coverage of only 5 pct. Theoretical Considerations The work of adhesion W is the energy bound (in ergs per sq cm) when an interface is formed. It is determined by, the difference of the free surface energies (surface tensions) of the respective phases ?1 and ? 2 before contact and the interfacial free surface energy ?12 after contact. The definition of the contact angle permits the elimination of the unknown surface energy of the solid and hence the calculation5 of W from the surface tension of the liquid ? and the contact angle ?: [W = y (1 + cos ?)[1]] Consider a surface consisting of two components, identified as 2 and 3, 1 being the liquid. The amount of 2 in the composite surface is x, where 0 < x < 1. The respective contact angles with 1 and air are ? and ?3. The total work of adhesion of such a surface is the sum of the values of the components multiplied by their respective areas. A formal relation can be written: [W,,,=x•W2+ (1-x).WR[2] .] in which Wm is the work of adhesion of the composite surface. Eq 1 can be introduced into W2 and W3 but in the case of Wm some discussion is needed. If the two components are segregated, each component forming an integral part of the composite surface there is no physical meaning for a contact angle ?m, calculated from Wm, by using eq 1. If, on the other hand, the area of each patch of the components is small in comparison with, say, the diameter of the bubble used in measuring, it could be expected that ?m would have aphysical significance, because of the action of the surface tension of the liquid-gas interface tending to smooth out sharp corners. How small these patches would have to be is difficult to predict, but by using composite surfaces with microscopically]

Jan 1, 1952

By O. J. C. Runnalls, L. M. Pidgeon

Some observations on the kinetics of the iodide process are reported. The deposition rate is geometry-sensitive in a system containing a finely divided titanium charge. Further, results indicate that the iodine diffusion rate influences the velocity of the process. The nonvolatile iodide, Til,, forms in the hot filament zone, thus removing iodine from the cycle. TITANIUM metal of 99.9 pct purity may be prepared using a refining technique originated by Van Arkel and de Boer.&apos; The purity of this metal, commonly called iodide titanium, exceeds that produced by any known process. In a recent application, the method was employed by Gonser et al.² to prepare titanium rods up to 2 to 3 cm in diam. In the Van Arkel-de Boer system, the relative influence of the fundamental mechanisms: l—production of titanium iodides, 2—gaseous countercurrent diffusion, and 3—decomposition, on the deposition rate have not been clearly established. Blocher and Campbell" have indicated that the controlling step in the process under practical conditions of operation may be the reaction rate of iodine with the crude metal. Fast&apos; reported that crude titanium metal reacted with iodine rapidly, even at room temperature, in his apparatus. Little has been reported on the effect of gaseous diffusion or decomposition on the deposition rate. It is these aspects of the process about which this investigation is centered. An attempt has been made to separate these latter effects from those due to the formation of the iodides at the crude metal surface by a division of the experimental program. Reaction of Iodine with Titanium Apparatus: In the investigation of gas-metal reactions of this type, the chemical reactivity of the halogen and halide vapors dictates the use of all-glass apparatus. In such a system standard techniques for measuring reaction rates are difficult to employ. Here, a simple apparatus was devised (Fig. 1) so that some indication of the reactivity of titanium powder with iodine vapor could be obtained. A stream of iodine gas was evolved from a bulb of controlled temperature and passed over a sample of titanium powder heated in a horizontal tube furnace. The product of the reaction, TiI4, volatilized and was condensed outside the furnace in a series of four glass bulbs, each cooled to room temperature in turn. Preliminary experiments indicated that distillation was retarded in a sealed evacuated system due to a pressure build-up in the condensing end of the apparatus. Hence, the system was pumped continuously using a mechanical pump and two oil diffusion pumps in series, through a liquid air trap. The iodine bulb was made large and a capillary restriction was inserted between the titanium bulb and the condensers so that the iodine pressure over the metal would approach the equilibrium pressure over solid iodine crystals. The effect of this restriction on the evaporation rate of TiI4, was determined separately. The iodine bulb was heated in an oil bath controlled to ±2°C. The titanium bulb temperature was automatically controlled to ±5°C. Procedure: About 200 mg of —30 mesh titanium powder, weighed to 0.1 mg, was placed in the reaction bulb after part B had been joined to part A. The powder was tapped into a long (5 cm) shallow mass along the bottom of the tube. Two chromel-alumel thermocouples were inserted into the magnesium radiator which was clamped to the reaction

Jan 1, 1953

By M. B. Bever, A. B. Michael

THE structure of cast A1-Si alloys is altered profoundly by modifying agents. Sodium, in particular, reduces the size of the silicon particles in the eutectic and tends to change their shapes from plates to nearly rounded grains. This refinement is accompanied by a shift of the eutectic to higher silicon concentrations and lower temperatures. Similar effects can be attained by rapid solidification. Hypotheses advanced to explain modification have involved the formation of a ternary eutectic,1 the removal of oxides by fluxing,&apos; and even a presumed allotropic transformation of silicon. Other hypotheses assume that the modifying agent causes an envelopment of the silicon particles by the aluminum-rich solid solution, but attribute this envelopment to different mechanisms. According to various explanations, the growth of the silicon particles is obstructed by an immiscible sodium-rich liquid," an adsorbed layer of sodium,&apos; or a ternary compound;5 his obstruction has been conceived as purely mechanical or as a colloidal action.&apos; It has also been proposed that sodium reduces the surface tension on the Al-Si interface, thus permitting the aluminum-rich solid to grow faster and to envelop the silicon particles.? Still other hypotheses stress undercooling and the attendant change in the rate of nucleation of silicon, but fail to ascribe any definite function to the sodium addition." &apos;" Procedure High-purity alloys of aluminum and 3 or 7 pct Si were treated with modifying agents containing radioactive sodium tracers. The experiments were intended to investigate the partition of sodium between the primary aluminum-rich solution and the eutectic, and, if possible, to determine whether sodium is concentrated in or around the silicon particles in the eutectic. Radioactive sodium fluoride, alone or mixed with stable sodium chloride, was allowed to react with the alloy for 5 min immediately before solidification in the crucible. Modification could not be attained with additions of less than the equivalent of approximately 0.1 pct Na. Some alloys were not completely modified, but comparison of the structures of treated and untreated specimens indicated a very considerable reduction in particle size of the silicon in all of the former. A treated alloy is shown in Fig. 1. Radioactive sodium fluoride was prepared by bombardment with deuterons having an energy of 14 mev. This bombardment (totaling, for example, 6 microampere-hours in one run) produced radioactive Na24 (half-life 14.8 hr) by the reaction 11Na23 (d,p) 11Na24. The radioisotopes of fluorine also produced have short half-lives and were not detected. A half-life determination by counting confirmed that the measured activity was due to Na24. The distribution of the sodium in the solidified alloys was determined by an autoradiographic technique by which a suitable stripping film is attached to a very thin metallographic specimen. After exposure and development, this emulsion remains superimposed on the specimen and may be examined microscopically or photographed by reflected light. The emulsion of the autoradiograph can be correlated directly with the underlying surface by simple adjustment in focus. The details of this technique have been described elsewhere." Results Fig. 2 is a micrograph of the autoradiographic emulsion ("autoradiograph") lying directly above the area of eutectic in Fig. 1. Fig. 3 shows a similar autoradiograph of a region consisting of primary solid solution. The small black dots (tracks) in these autoradiographs are developed grains in the emul-

Jan 1, 1954

By T. R. Ingraham

When aluminum sulfate was decomposed in an evacuated apparatus and the sample cooled, Q alumina was found. The thermodynamics of the decomposition reaction were resolved by measurements of the total pressure of SO3, SO2, and O2 generated over the sample at various temperatures. The results were correlated with other published data to calculate the rmges of thermodynamic stability of the various compounds involved. The thermal decomposition of aluminum sulfate was studied by Wijhler, Pluddeman, and Wöhler1 and by Warner and Ingraham.2 The results of both studies were critically reviewed by Kellogg,3 who observed that "each set of data shows considerable scatter and strong curvature on a plot of log pso3 vs 1/T".3 He agreed with Warner and Ingraham2 that both the discrepancy in the two sets of results and their curvature may arise from the indefinite properties of the particular form of A12O3 which is formed during the decomposition. While studying the thermal stability of other sulfate systems, we had noted the presence of nonequilibrium oxide properties in both the cobalt4 and manganese5 systems, but neither had shown any appreciable curvature on a logPSO, vs 1/T relationship, and the data from both systems agreed reasonably well with prior work. It therefore seemed reasonable to reexamine the technique which had been used in our earlier work on aluminum sulfate.2 The principal difference was that a tightly compacted pellet had been used for the earlier aluminum sulfate work, whereas a loose powder, contained in a platinum boat, was used for our work on other sulfate systems. In addition, a better technique had been developed for dehydrating the samples. From work done on the nickel system,6 we had become aware of the highly protective nature of some sulfate layers on their oxjdes, and hence of the necessity of providing a large surface area of P3e sample when equilibrium was to be attained in a reasonable time. That observation suggested that perhaps a steady state, rather than equilibrium, had been reached in the earlier work on aluminum sulfate. This paper reports a repetition of the experimental work with large, finely divided samples of anhydrous aluminum sulfate. APPARATUS AND PROCEDURE The apparatus used in the experimental work was described in earlier papers.2,7 The source material was Anachemia reagent-grade Al2(sO4)3 - 18H2O which was first partly dehydrated by heating at 400°C for 48 hr and then completely dehydrated by repeated baking of an aluminum sulfate-oleum slush to dryness at 450°C. ? Alas was prepared by decomposing some of the sulfate in a muffle furnace at 800° C overnight. Approximately equal amounts of the 7) alumina and aluminum sulfate were used in the experiments. The finely divided samples were handled under dry box conditions, and in addition some of the aluminum sulfate was decomposed in the apparatus while it was under vacuum, to ensure its complete dehydration prior to sealing the apparatus. The samples were heated to a series of constant temperatures on both increasing- and decreasing-tem-perature programs. Two to three days were required to obtain steady readings of the total decomposition pressure on an increasing-temperature program, and 5 to 6 days on a decreasing-temperature program. Three samples were examined on both programs. Within experimental error, the results for each sample and each program could not be distinguished.

Jan 1, 1969

By Donald Ofte, L. J. Wittenberg

The absolute viscosity coefficients and activation energies for viscous flow of bismuth, lead, and zinc are reported. The viscosities were measured in an oscillating cup viscosimeter from nearly 1000°C to within 1 deg of the melting point of zinc; 2 deg of the melting point of lead; and in the supercooled condition of bismuth, 9 deg below the melting point. Two methods of relating the change in the viscosity coeflicient with temperature were compared. From the plot of the logarithm of viscosity (77) as a function of reciprocal absolute temperature (1/T), the equations of the lines which fit the data are: AS a part of the Reactor Fuels and Materials Research program at Mound Laboratory, precise measurements of the physical properties of liquid metals are of interest because the desirability for a low vapor pressure liquid coolant in high-temperature nuclear power plants has focused attention on the properties of the liquid metals.&apos; Also, a clearer understanding of the liquid metal state can be achieved when better measurements are available. For these reasons, the viscosity values of certain liquid metals have been determined. The viscosities of the liquid metals, bismuth, lead, and zinc are measured in an oscillating cup viscosi-meter. In this apparatus the liquid is sealed in a right-circular cylindrical cup which is attached to a torsion fiber so that the system forms a torsion pendulum. The damping effect of the molten metal upon the normal oscillations of the torsion pendulum is a function of the viscosity of the liquid. This method is advantageous because of the small amount of sample required (8 to 10 cc), the ease of remote operation of the apparatus in a vacuum system, and the containment of the liquid metal in a hermetically sealed, nonreactive, tantalum crucible. With the liquid metal sealed in the crucible, loss of liquid by vaporization and chemical reactions with atmospheric gases are prevented. Additionally, an absolute viscosity determination is obtained which avoids the sources of possible error in a relative measurement. The difficulties in a relative method include the repetitious cup calibrations, and the uncertainty inherent in the practice of calibration of the apparatus at room temperature and extrapolation to the high temperatures necessary for the investigation of most liquid metals. The oscillating cup viscosimeter was first described by Meyer in 1891.2 The first complete mathematical treatment offering an absolute measurement of viscosity with this type of apparatus was proposed by Andrade and chiong3 in 1936 for an oscillating sphere filled with a liquid. This solution was modified to include a right circular cylinder by Hopkins and Toye4 in 1950, and R. Roscoe5 in 1958. Roscoe&apos;s treatment for the calculation of the viscosity of a liquid at a particular temperature from the logarithmic decrement and period of oscillation of the torsion pendulum was used in this investigation. A detailed description of the method of calculating the viscosity from these measurements has been reported earlier.&apos; This calculation has been programmed for the IBM 704 and IBM 1620 computers for expedition of the otherwise laborious calculations. APPARATUS The cutaway view of the apparatus in Fig. 1 shows the suspension system within the high vacuum enclosure. The low residual gas pressure. maintained between 1 x 10-4 and 5 X 10-6 mm Hg during a determination, avoided both air drag on the pendulum and

Jan 1, 1963

By J. W. Downey, J. B. Darby, L. J. Norton

THE only previous investigation of the phase equilibria in the Ta-Pd system was reported by Greenfield and Beck.1 Their work (actually a portion of a much broader survey) was limited to the composition range 50 to 75 at. pct Ta and to a single temperature, 1000°C. The results indicated that no intermediate phases were present at this temperature. They pointed out that this was an unexpected result in view of the fact that niobium, which belongs to the same group in the periodic table as tantalum and has essentially the same atomic size, forms a o phase with palladium.&apos; Also, tantalum in combination with rhodium,&apos; iridium,&apos; or platinum&apos; stabilizes the s phase. By analogy, the Ta-Pd system would also be expected to contain a s phase. The present investigation was therefore undertaken to explore more fully the phase relationships in this system. Alloys were prepared by arc melting on a water-cooled copper hearth in an argon-helium atmosphere. The purity of the starting materials was greater than 99.9 pct. The weight losses on melting were less than 1 pct and therefore the alloys were not analyzed chemically. Specimens were wrapped in molybdenum foil, encapsulated in quartz capsules under a vacuum of at least 1 x 10-5 mm of Hg, annealed as indicated in Table I, and water quenched. Optical and X-ray metallography were used for identifying the phases present in the annealed and quenched alloys. The alloys were resistant to attack by several acids; however, a sodium cyanide electroetch and an immersion etch containing 1 part HF, 1 part HNO3, 2 parts H2SO4, and 5 parts H2O by volume were found satisfactory. The X-ray diffraction patterns were taken with a Straumanis-type Debye-Scherrer camera and filtered copper or chromium radiation. A summary of the phases found in this investigation is presented in Table I. No attempt was made to determine the composition limits of the various phases. The present results indicate that this system consists of two terminal solid solutions separated by at least four intermediate phases at the approximate compositions Ta3Pd, -TaPd, TaPd,, and TaPd3. The Ta-rich solid solution, containing less than 10 at. pct Pd at 1150°C, is in equilibrium with a o phase which is stable in the vicinity of 25 at. pct Pd. The latter phase is also in equilibrium with a bct phase at the equiatomic composition. At high temperatures it appears that the Pd-rich solid solution extends to at least 66.6 at. pct Pd and is in equilibrium with the bct phase. When annealed at 900°C, a sample containing 66.6 at. pct Pd transformed to an unidentified phase designated as X. An X-ray diffraction pattern of this phase contained sharp low-angle lines while the high-angle lines were characteristically diffuse. The observed d-spacings and relative intensities for lines in the low-angle region are presented in Table 11. In the vicinity of 70 at. pct Pd an intermediate phase having the TiA13-type structure is formed. It is stable to at least 1100°C, and presumably dissolves congruently into the ter-

Jan 1, 1963

By J. F. Gormley

Drill pipe, and the connections used to join the pipe together, have had a long history of development and improvement. With the growing use of high tensile-strength pipe, the rotary shouldered connections used to join the lengths of drill pipe have become more critical. Fatigue-type failures of rotary-shouldered connections, or tool joints, have become a cause of much conern to operators and manufacturers. Most fatigue tests on tool joints have been made on the basis of bending moment applied vs number of cycles, rather than on the basis of stress vs cycles. A desire to learn more about the nature of stress in a tool joint due to bending caused a rather intensive experimental study to determine what actually happens to cause fatigue failure. It was known that a tool joint with insufficient make-up torque was subject to early fatigue failure. Therefore, the establishment of the relationship between make-up torque and allowable bending moment would enable a testing engineer to better correlate the results of various tests. The problem of calculating the stress in a tool joint due to an applied bending moment was complicated by: the effect of unknown stress concentrations; the applicability of the well known formula S = Mc/I; and the question of whether to use the combined cross section of the pin and box in calculating the moment of inertia I. TEST EQUIPMENT The test equipment consisted of the following. 1. A lathe modified to act as a fatigue machine for full-size tool joint or drill-collar specimens. 2. An adapter plate bolted to the headstock of the lathe and into which a short adapter was screwed. 3. Tool-joint pins on sections of drill collars bucked into the adapter. 4. A hydraulic load cylinder which rested on the bed of the lathe and applied bending moments to the joints. 5. Paper-backed strain gauges (FAP-12-12, 1/8-in. gauge length and A-5-1, 1/2-in. gauge length). 6. Eastman 910 contact cement for bonding gauges to joint and Epoxylite 222 waterproofing. 7. A 12-position switchbox, SR-4 bridge balancing unit connected to an SR-4 strain indicator to read the gauge output. 8. A four-channel Sanborn recorder, Model 150, was used as the readout instrument for part of the testing. The fatigue machine was well suited as a loading device. Because of the long lever arm available, the change of moment with distance was small; consequently, the vertical shear stress was small, less than 300 psi. Some difficulty was experienced with the hydraulic load cylinder at high bending moments due to leakage. The strain gauge equipment was simple and quite reliable. A 41/2-in. extra hole (E. H.) joint with "as machined" threads and shoulders and a 2 7/8-in. internal flush (I. F.) joint with copper-plated threads and shoulders were selected for testing because of their common usage in the field. In addition, the 4 1/2-in. E. H. was suitable because it had an inside diameter large enough to permit the insertion and accurate positioning of strain gauges without using special jigs, while the 2 7/8-in. I. F. joint required much lower bending loads to cause separation of the shoulders of the joint when made up to the recommended torque. The joints were made to standard API specifications, except for very small bevels on the box and pin shoulders and cylindrical stress-relief grooves added to the pins. Larger bevels would have

By P. Payson

Intergranular corrosion in corrosion-resistant chromium-nickel steels has been widely discussed in the last few years. So far as the author knows, nothing has been published which definitely shows that this tendency can be eliminated, although suggestions have been made that a remedy is possible if certain specifications are satisfied. Strauss, Schottky and Hinnüberl suggested an increase in chromium content to an extent that would prevent the impoverishment of chromium on carbide precipitation sufficient to cause impaired corrosion resistance in the matrix. Pilling2 suggested an increase in nickel, so that the stability of the austenite matrix would be increased. Aborn and Bain3 say that "intergranular attack—may be eliminated by preventing carbide precipitation (e. g., by lowering the carbon content or somehow raising its solubility) or by precipitating it permanently under conditions which will not remove chromium from solid solution so drastically at any points." In a later paper Aborn and Bain4 state that many different metallic elements, tungsten, vanadium, copper, aluminum, molybdenum, titanium and zirconium, have been added in small percentages to increase the stability of these alloys, but that it has been reported that according to the copper sulfate test these added elements act only to retard the intergranular corrosion. and that increased nickel and chromium contents have similar effects. Newell5 showed that the lower the quenching temperature before reheating, the less severe was the intergranular attack.

Jan 1, 1932

By W. G. Matteson

THE origin of the salt domes of the Gulf coastal plain has been investigated by many of the most able geologists, but the problem cannot be said to have been satisfactorily solved. Since 1860, numerous theories have been presented, only to be discarded, at least in part, as more complete information revealed their fundamental weakness. Real progress toward solution dates from 1902, when Hill&apos; advanced the theory of secondary deposition of the domal materials from saturated solutions of hot saline waters ascending from great depths under hydrostatic head along structural lines of weakness. Shortly thereafter, Harris,2 using Hill&apos;s hypothesis as a basis, explained the doming and pronounced uplift associated with these salt cores as the result of forces exerted by growing salt crystals. This was a marked advance over the ideas of Coste3 and Hager,4 since no. evidence of igneous intrusives, as they assumed to explain the uplifts, had been found associated with the domes. Harris5 developed his theory until it offered such apparently plausible explanations of so many details of dome phenomena that his hypothesis and conclusions received widespread acceptance, despite some serious objections, and today his theory, somewhat modified, is considered by many able investigators to be the best explanation of, the origin of these domes. The immense production of oil per acre, the recognition of the high lubricating quality of the oil, the development and recognition of the efficiency and advantages of oil-burning vessels, with the, subsequent

Jan 2, 1921

By N. B. Pilling

The deleterious effect on the mechanical properties of copper, re-sulting from heating in contact with reducing gases, is well known, but the mechanism of the action does not appear to have been definitely established. The purpose of the present investigation was not to determine the exact variations in physical quality of commercial copper, with its various impurities, as dependent upon the composition of the gas, temperature of exposure, etc., but rather to study the nature of the action and the conditions under which it occurs. The physical result of the so-called "gassing" of copper has been generally described as the development of "brittleness." There appears to be a striking decrease in tensile strength, associated with a considerable loss of ductility, and a small copper strip or wire affected in this way can be snapped in two when bent. Larger articles may have an outer layer alone affected, which can be detached from the core by hammering or bending. Perhaps the earliest reference to this subject is that of Heynl in 1900, and among the later observers may be mentioned Archbutt,2 Bengough and Hill,3 Johnson,4 Mathewson and Thalheimer,5 and Ruder.6 Bengough and Hill, while working with arsenical copper, were the first to suggest the possibility of the formation of gases within the copper itself, while Ruder endeavored to explain the action by the reduction of the

Jan 1, 1919

By W. R. Shimer

(New York Meeting, October, 1913.) THE investigation herein described was carried out for the purpose of studying, both by chemical and metal-lographical means, the extent of over-oxidation of steel that can be accomplished by excessive over-blowing in a Bessemer converter. In addition there are appended some results of basic. open hearth and crucible steels. Remarks on Chemical Methods. The test block used was hemispherical in shape, 4.5 in, in diameter and 2 in. thick. Drillings for analysis were obtained by drilling through the entire solid part of the. block, carefully avoiding all cracks anti blow-holes and mixing these drillings thoroughly. Drillings were carefully examined for scale and the finest were gone over with a microscope to be sure all scale from whatever source had been. removed. Oxygen was determined by the well-known method of Ledebur, modified according to Cushman,1 with, however, the removal of the preheating tube, which was found unnecessary. This method has been found to give concordant results. Blanks run from 0.0003 to 0.0006 g. Duplicate determinations varied not more than 0.001 to 0.003 per cent. It seems to be generally supposed that the hydrogen method gives only that oxygen which is combined with iron. Whether this be true or not, the content of oxygen existing as iron oxide no doubt predominates sufficiently, so that the result obtained is sufficient to indicate whether the steel is over-oxidized or not.

Jan 9, 1913

By Robert Schorr

PAGE 1. Introduction,........... 82 2. Characteristics of Briquettes,........ 87 3. The Manufacture of Coal- and Coke-Briquettes,.... 89 Binders, Organic and Inorganic,...... 90 Mixing,...........94 Presses, Continuous and Intermittent Action,....95 Cost of Briquettes and Sales-Prices in Various Countries,.. 99 4. The Manufacture of Peat-Briquettes,......101 Solid Peat-Slabs,.........101 Solid, Carbonized Peat-Briquettes,......103 Estimates of Cost of Operating Peat-Briquetting Plants,... 105 5. Manufacture of Mineral-Briquettes for Metallurgical Processes,.. 108 6. Manufacture of Artificial Stone-Masses,......112 7. Bibliography,...........115 Introduction. Briquetting is apparently a very simple operation, yet it has offered so many mechanical and chemical difficulties that it required almost a century to place it on a commercial basis. Since 1860, however, the progress has been steady and satisfactory, and to-day, for most of the European coal companies, the briquette-plant is a very profitable investment. Among the many applications of scientific knowledge to further economy by recovering and utilizing by-products and raw materials, there is possibly none which deserves the attention of Americans to a higher degree than briquetting. The recent miners&apos; strike in Pennsylvania, which resulted in a scarce and irregular supply of coal at a high price, has advanced the possibilities for briquetting, and as a consequence public interest has grown rapidly. While the manufacture of coal-briquettes is not new in the United States, adverse conditions and sometimes lack of

Jan 1, 1905

By Robert T. Hill

The successful completion, January 10,1901, by Capt. A. F. Lucas, of a well, near Beaumont, Texas, whereby an enormous flow, estimated at &apos;75,000 barrels a day, was obtained, opened a new oil-field in the United States, kindled a frenzy of exploitation and speculation, revolutionized the fuel industry of a large region, and brought gain to thousands of people. Even to-day, it is impossible to cast up the present results or to prognosticate the future influence of this event. It has caused the revival of attention in other localities where oil had been suspected, and exploration for oil throughout the Texas region. It has attracted notice to the mineral resources of the Texas region, and created an interest in the geological conditions of that great State. This State, which has increased in population and wealth, as recorded by every succeeding census, with leaps and bounds such as are exhibited by no other part of the Union, now stands fifth in population and first in productive wealth per capita. Its fields, pastures, forests and mines teem with raw material. The whole economic evolution of the State has gravitated toward a focal point where these products were available for the coming of the kiln, the machine and the factory. The only drawback to the prosperity of the State was the lack of an economic fuel, inferior coal costing an average of $5.00 per ton at the time of the Beaumont discovery. This

Jan 1, 1903

By P. Ramachandrarao, T. R. Anantharaman

CONSIDERABLE interest has lately been evinced as regards the nature of chill zones in solidified metals and alloys. Biloni and Chalmersl were the first to show through their study of segregation substructures in some nonferrous alloys that the formation of the dendritic region may be preceded by a diffusionless solidification process, viz., predendritic solidification. Subsequently Bower and Flemings2 tried a special solidification technique wherein the liquid was drawn into a narrow copper mold with polished surfaces and concluded that convection might trigger some multiplication mechanism leading to grain refinement. Using uncoated and partially coated surfaces for molds in the Bower-Flemings technique as well as in conventional molds, Biloni and Morando3 have very recently brought out the importance of the rate of heat extraction on the mechanism of solidification. We report here on the surface structures and substructures observed in a Sn-1 wt pct Pb alloy solidified at even higher cooling rates (riz., l05 to l07 ºc per sec) than those employed by earlier workers. The alloy was made by melting tin (99.99+ pct) and lead (99.9+ pct) in a silica tube under vacuum. Small quantities of the homogenized alloy (0.5 to 1.0 g) were then quenched (or splat-cooled) from the melt by the "gun technique" developed by Duwez et al.4 The thickness of the resultant foils varied from specimen to

Jan 1, 1970

By Cyril Stanley Smith, Earl W. Palmer

A STUDY of the precipitation-hardening of copper steels1 led the authors to investigate malleable iron containing copper, for the low-carbon ferritic matrix in malleable iron should lend itself admirably to precipitation-hardening. It was soon found that in addition to rendering malleable iron susceptible to improvement by precipitation-hardening treatments, copper has another potentially useful effect as an accelerator of graphitization. Brief mention of these effects was given in a general paper by Lorig and one of the present authors2; the present paper gives further details on the graphitization and precipitation-hardening effects only. After the completion of this work a paper by L. Lykkin3 appeared, confirming the authors&apos; conclusions regarding graphitization. MATERIAL USED After some preliminary heats had been made in the laboratory to determine the effect of copper, several castings from commercial air-furnace heats were obtained, and data from these alone are given here. Part of the metal was poured directly and part was treated in the ladle with the desired amount of copper before pouring. Green-sand molds were used, each holding two tensile test pieces of the form adopted by the Malleable Iron Research Institute, or two bars for graphitization studies, 5/8 in. in diameter and 9 in. long, fed through two enlarged sections equidistant from the middle and ends of the bars. Risers of suitable size insured sound castings. Tensile tests were made

Jan 1, 1935