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By G. P. Tiwari

Recrystallization and grain growth in thoria dispersed nickel and nichrome were recently studied by Webster as a function of temperature and deformation. The unexpected part of these results was that specimens which had received heavier deformation developed greater resistance to recrystallization. Retardation of recrystallization was accompanied by the formation of voids around thoria dispersion. To explain these results, Webster suggested that the formation of void around the particles increased the effective size of thoria particles. This resulted in greater impediment to the grain-boundary migration and as a consequence the recrystallization of the matrix is retarded. In the present note an alternative and more probable explanation for the effect of voids on recrystallization is presented. The exact mechanism of void formation in thoria dispersed nickel or nichrome is not known. However, it is reasonably certain that it must be preceded by the stress concentration in the matrix around thoria dispersion during the deformation.'' The resulting stress concentration must be sufficient enough to supply the surface energy for the new surfaces created. Further, the decrease in the strain energy of the matrix surrounding the potential void nucleus must be larger than the surface energy of the newly created surface. The release of strain energy due to formation of crack results in a strain free cylinder of the material around the voids.13 If the void formation is not localized, at few points only (as is the case here), this process may lead to considerable amount of release of strain energy of the matrix. The pattern of recrystallization behavior of single phase homogeneous matrix as well as the matrix having a second phase dispersion is same except for the fact recovery and recrystallization are more clearly delineated.14 In general, the recrystallization temperature is lowered (i.e., recrystallization is easier) with increase in the amount of cold work. This is due to the increase in stored energy in the matrix with increasing amount of deformation. If somehow there is a relaxation of strain energy in the matrix, the recrystallization should become difficult because of the decrease in the amount of stored energy available for recrystallization. Since the formation of voids leads to a decrease in the strain energy of matrix, the recrystallization of the matrix would be inhibited due to the formation of voids during deformation prior to recrystallization. It has been observed by earlier workers15'16 that the presence of preexisting voids in a matrix retards the recrystallization. The essential issue here is how do the voids act to produce this effect. If the voids influence recrystallization only by blocking the grain boundary migration, then the effect should be maximum when they are present almost exclusively along grain boundary. These conditions are obtained during high temperature deformation. However, the voids produced due to creep along grain boundary are not able to prevent recrystallization17 suggesting that they are not effective in blocking grain boundary movement. Recently it was shown by Davies and Williams that the voids can act as sinks for vacancies." As a result the processes dependent on vacancy diffusion like recovery, recrystallization, dislocation climb, and so forth, will be hindered. This fact may be responsible for inhibition of recrystallization during subsequent deformation and annealing cycles. It is to be noted here that there is a large difference between the density of voids in creep experiments and the other experiments where retarding effect of voids on recrystallization is seen. The voids in former may number up to l04 to l05 per sq cm whereas in latter cases the voids density is typically around 1010 to 1013 per sq cm. It appears that the decrease in supply of vacancies in creep is insufficient to adversely affect the recrystallization due to low void population. The author is grateful to P. Das Gupta and S. P. Ray for helpful discussions. Author's Reply D. Webster Tiwari appears to have misunderstood the nature of grain boundary-particle interactions. Tiwari (quoting Cahn) states that second phase particles become more effective as they become smaller, therefore as the voids in TDNiC make the thoria particles effectively bigger their ability to resist grain boundary movement is impaired. This particle size argument was originally proposed in the form of an equation by Zener 20 years agol9 and is not necessarily valid as is discussed below. However, assuming it is valid, it predicts a greater boundary restraining effect by smaller particles simply because their combined cross sectional area is greater at a constant volume. If the number of particles remains the same and their effective size increases, as in the present case, Zener's equation predicts a greatly reduced grain size. This is because the effect

Jan 1, 1970

By D. J. McAdam

In a series of papers the author and associates have discussed the influence of temperature on the tensile properties of metals.11-18 These papers present much information about the influence of temperature and the stress system on the conventional indices of mechanical properties, with special attention to the fracture stress. A recent study of the data, however, has revealed much additional information about the influence of temperature on the fundamental factors involved in the flow of metals. The present paper presents results of this study. Attention will be confined almost entirely to results derived from tension tests of unnotched cylindrical specimens at strain rates a little slower than those used in ordinary tension tests. According to a concept first presented by Ludwik and elaborated in recent papers by others,8,9,22,23 the mechanical state of a metal depends on the total plastic strain, but not on the temperature during straining, provided that the only structural changes are those essential to plastic deformation. In the summer of 1948, however, the author made the previously mentioned study of results of a general investigation by the author and associates and reached the conclusion that the mechanical state depends not only on the total strain, but also on the temperature during the straining. A number of diagrams were then prepared. These conclusions were presented without diagrams in a discussion last October of a paper by Dorn, Goldberg and Tietz.2 The metals used in the investigation on which this paper is based were Monel and oxygen-free copper. The Monel was supplied by the International Nickel Co. through the courtesy of Dr. W. A. Mudge. The copper was supplied by the Scomet Engineering Co. through the courtesy of Dr. Sidney Rolle. The data to be presented are based on results of tests at temperatures ranging between 165 and — 188°C. Description of the apparatus and methods of test are given in previous papers.1011'1"2 The present paper is the first part of the general discussion of the influence to temperature on the stress-strain-energy relationship for metals. The next paper will deal with metals that are subject to structural changes other than those induced solely by plastic deformation. Influence of Temperature and Plastic Strain on the Flow Stress of Monel and Copper For a study of the influence of temperature on the stress-strain relationship, flow-stress curves obtained with annealed metals at various temperatures will be compared with curves obtained with the same metals after cold drawing or cold rolling at room temperature. Diagrams thus obtained with Monel and copper are shown in Fig 1 to 8. Fig 1 to 7 show the variation of the flow stress with temperature and plastic strain; Fig 8 is a diagram of a different type, derived from Fig 4 to 7. In Fig 1 to 7 strain is expressed in terms of A0/A, in which A0, and A represent the initial and current areas of cross-section. Since values of Ao/A are represented on a logarithmic scale, abscissas are proportional to true strains; moreover, the true strains representing prior plastic deformation and those representing subsequent strain during a tension test are directly additive. Fig 1 shows flow-stress curves obtained with annealed Monel. Five of the curves are based on results of tension tests. Between yield and the maximum load, the flow was under longitudinal tensile stress; between the maximum load and fracture, the local contraction induced transverse radial tensile stress. The portions of curves designated F, therefore, represent flow with increasing radial stress ratio, the ratio of the transverse stress S3 to the longitudinal stress Si. Curve Fo is based on the ultimate stresses of specimens taken from bars that had been cold drawn various amounts.17 Since the tensile stress at the maximum load is unidirectional, curve Fo represents the course that a flow-stress curve would take if the stress during an entire tension test could be kept unidirectional. The flow-stress curve F obtained at room temperature (Fig 1) has been established accurately by numerous measurements of the diameter of the specimen during the extension from yield to fracture.17 At the time of the experiments, however, no apparatus was available for measuring the diameter during tension tests at low temperatures. Nevertheless, curves have been established to represent with sufficient accuracy the flow at low temperatures. Each flow-stress curve must be tangent to a curve U, which starts at a point representing the ultimate stress of annealed metal. Since the ultimate stress is based on the area of

Jan 1, 1950

By A. E. Desrosiers, R. L. Kathren, D. L. Haggard, J. M. Selby

INTRODUCTION The radiological health significance of thorium-230 stems from its tendency to separate from the uranium238 parent, concentrate in bone tissues, and to subsequently irradiate the radiosensitive tissues lining the bone surfaces and the bone marrow. Indeed, thorium-230 may be the radionuclide which contributes the major dose following intake of natural uranium (Hartley and Pasternack 1979). This is reflected by the most recent recommendations of the International Commission on Radiological Protection, which specify the limits shown in Table I for the annual intake of radionuclides by occupationally exposed workers (ICRP 1979). TABLE 1. Occupational Annual Intake Limits (microcuries per year) for Selected Uranium Nuclides and Daughters (ICRP 79) [Radionuclide Ingestion Inhalation] [Uranium-238 200 0.05 Uranium-235 200 0.05 Uranium-234 200 0.03 Thorium-234 300 200 Thorium-230 3 0.02 Radium-226 2 0.5] Clearly, the relatively low annual limit of intake for thorium-230 shows it to be of greater radiological concern than its parent radionuclides. Because of the greater toxicity and different metabolism of thorium-230, monitoring only for uranium-238 does not satisfactorily identify the possible hazard from thorium-230 nor does it provide any real indication of the metabolism or biodynamics of these two radionuclides. Thorium-230 has a half-life of 80,000 years and can be detected by direct counting of the alpha particles or photons emitted during its transformation to radium-226. The 4.69 and 4.62 MeV alpha particles are distinctive and specific indicators of thorium-230 and are emitted with abundances of 76% and 24%, respectively. The principal photon, a 68 keV gamma ray, is emitted in only 0.37% of the transformations and is, therefore, not useful for low level measurements. The other photons emitted have even lower yields, or, in the case of radium L x-rays, are non-specific and, hence, useless for quantification. High sensitivity measurements of thorium-230 currently are usually accomplished by wet washing of the sample substrate, quantitative chemical separation of thorium atoms, and, finally, direct measurement of the alpha particles emitted from a massless deposition. This procedure is complicated, expensive, and time-consuming, and subject to interferences from uranium, other actinides, and other thorium isotopes. Recently, the feasibility of low-level measurement of thorium-230 by neutron activation analysis (NAA) was demonstrated (Kathren, Desrosiers and Church 1980). Two principal variations of the NAA method were used in this study: 1) instrumental NAA technique and 2) post-irradiation radiochemical separations (RCS). Instrumental NAA procedure is a nondestrucive technique which is preferred because of its simplicity. The procedure is as follows: after irradiation with a known neutron fluence, the samples are transferred to a clean container and quantitative gamma spectroscopy performed. With the radiochemical separations procedure, the sample is initially treated as in the instrumental technique. However, after irradiation, a known amount of "carrier" is added to the sample. The element(s) of interest are then separated from the rest of the matrix by distillation, precipitation and extraction techniques. The resulting sample, now free of interferring elements, is then ready for gamma-ray analysis. The use of a "carrier" is to determine the loss of element-of-interest during the chemical separations process. The neutron activation cross section of thorium-230 has an epicadmium resonance value of 1,010 barns (Mughahghab and Garber 1976) and a thermal neutron cross section of 23 barns. The 25.52 hr thorium-231 produced releases two photons of significance: an 84 keV complex, (6.5% yield) and 25.6 keV (15% yield) (Lederer and Shirley 1978). The 84 keV complex is particularly useful for quantification since neither natural uranium, thorium, their daughters, or activation products emit photons in this region. However, the higher yield of the 25.6 keV photon may result in increased sensitivity if there are no other photons of similar energy emitted by other radionuclides in the sample. PRELIMINARY STUDIES Thorium-230 standard stock solution was prepared from a pure sample of the oxide purchased from Oak Ridge National Laboratory. From this stock solution a series of samples were prepared for irradiation in the TRIGA Mark I reactor at Reed College. Various dilutions were prepared as well as thorium-230 spiked urine samples. Irradiation times varied from 1 to 54 minutes in a neutron fluence rate of 1.84 x 1012 n/ cu m-sec. The neutron spectrum was abundant in thermal neutrons, having a Cd ratio of approximately 10. Treated urine samples were also analyzed by the NAA instrumental method. Analysis of untreated urine samples was not possible due to the high background

Jan 1, 1981

COUNCIL AND STANDING COMMITTEES - 1973-1974 Office Bearers: P. W. J. van Rensburg (President), Professor R. P. Plewman and Dr R. E. Robinson (Vice Presidents), J. K. E. Douglas (Honorary Treasurer), and Dr J. P. Hugo (Immediate Past President). Elected Members of Council: Dr M. G. Atmore, G. H. Grange, Dr P. R. Jochens, J. G. Kirchner, Dr D. I. Legge, W. W. Malan, Dr M. D. G. Salamon, L. W. P. van den Bosch, D. A. Viljoen, P. A. von Wielligh. Branch Chairmen: B. T. Hosking (Witbank-Middelburg Branch), E. T. Wilson (Orange Free State Branch). Past Presidents Serving on Council: R. J. Adamson, M. Barcza, H. Britten, H. E. Cross, Professor J. de V. Lambrechts, R. C. J. Goode, Professor D. D. Howat, D. M. Jamieson, D. G. Maxwell, Dr J. T. McIntyre, V. C. Robinson. Ten Council meetings were held during the year, with an average attendance of 19, and the standing committees held 30 meetings. COMMITTEE CHAIRMEN Membership, Dr R. E. Robinson ; Metallurgical Colloquia, Dr R. E. Robinson ; Mining Colloquia, L. W. P. van den Bosch; Awards, P. W. J. van Rensburg; Excursions, P. A. von Wielligh; Dinner, G. H. Grange ; Constitution, Rules and Policy, Dr J. P. Hugo; Adjudicating, P. W. J. van Rensburg; Mines and Works, W. W. Malan; Education, Dr J. P. Hugo. REPRESENTATIVES ON OTHER BODIES Associated Scientific and Technical Societies: Members : V. C. Robinson and D. G. Maxwell Alternates : P. W. J. van Rensburg and Dr J. P. Hugo. Federation of Societies of Professional Engineers Members : J. K. E. Douglas and P. W. J. van Rensburg Alternates : Dr J. P. Hugo and G. H. Grange. South African Council for Professional Engineers Members : R. C. J. Goode and J. K. E. Douglas Alternates: G. H. Grange and Dr R. E. Robinson. Engineers' Liaison Committee (Pretoria): Member: Professor J. de V. Lambrechts Alternate : Dr J. P. Hugo. MEMBERSHIP Seventeen Fellows and Members, twenty-three Graduates, ten Associate Members, twenty-two Associates, thirty-four Students, and seven Company Affiliates were elected during the year. Eleven Fellows and four Members were admitted to retired membership. Five Fellows were elected to Honorary Life Membership. Four Members, two Graduates, and one Student were transferred to Fellows ; eleven Graduates and Students were transferred to Members ; eight Students to Graduates; and four Students to Associates. A statement of membership as at June 30th 1974 and the end of the previous year is given in the following tabulation 30th - 30th June, - June, 1973 - 1974 Honorary Life Fellows 4 - 9 Honorary Fellows 9 - 8 Life Fellows 177 - 170 Fellows 536 - 544 Members 487 - 512 Associate Members - - 10 Graduates 128 - 130 Associates 186 - 194 Students 183 - 173 Company Affiliates 64 - 70 1 774 - 1 820 OBITUARIES Your Council records with deep regret the death during the year of the following members : Dr P. N. Lategan and Dr O. A. Jackson, Honorary Life Fellows and Past Presidents; C. Airth, T. L. Blunt, J. B. Dennison, A. E. Frazer, C. L. Lamb, V. O. Reid, K. Richardson and D. G. Roberts, Life Fellows ; H. F. Allan, J. T. Beaumont, M. Eisenstein, J. C. Hall, C. F. Louw, H. H. McGregor, R. Murchison, and J. E. Williamson, Fellows; and R. B. Miles, Associate. FINANCE The annual accounts, which follow this report, reflect a healthy position and show that measures taken by Council over the last few years to boost income have been successful. A higher income was needed not only to meet rising costs but also so that the services provided by the Institute for its members could be expanded. This year's income of R55 025 showed a further increase compared with last year's figure of R48 307. Income from subscriptions was higher mainly owing to an increased number of Company Affiliates, and this is indicative of the support given by mining and metallurgical companies to the good work being done by the Institute. Further sales of publications of the symposia held over the last few years again made a useful contribution to income of R4560. The first Winter School held in 1973 yielded a surplus of R7495 after the expenses had been deducted from the income received from registration fees. The cost of administering the Institute increased by R2212 compared with the previous year. Included in this was a donation of R1000 to the A.S. & T.S. Trust Fund. The cost of publishing and printing the Journal increased by R2034, but advertising and extraneous sales of the Journal were higher, with the result that the net cost of the

Jan 10, 1974

COUNCIL AND STANDING COMMITTEES, 1974-1975 Office Bearers : Prof. R. P. Plewman (President), Dr R. E. Robinson and Dr M. D. G. Salamon (Vice Presidents), J. K. E. Douglas (Honorary Treasurer), and P. W. J. van Rensburg (Immediate Past President). Elected Members of Council: Dr M. G. Atmore, E. Collier, G. H. Grange, Dr P. R. Jochens, Dr D. I. Legge, D. G. Malan, C. T. Shaw, L. W. P. van den Bosch, D. A. Viljoen, H. M. Wells, P. A. von Wielligh. Branch Chairmen: B. T. Hosking (Witbank-Middelburg Branch), D. A. Smith (Orange Free State Branch). Past Presidents Serving on Council: R. J. Adamson, M. Barcza (until May 1975), H. Britten, H. E. Cross, Prof. J. de V. Lambrechts (until December 1974), R. C. J. Goode, Prof. D. D. Howat, Dr J. P. Hugo, D. M. Jamieson, D. G. Maxwell, Dr J. T. McIntyre, V. C. Robinson. Ten Council meetings were held during the year, with an average attendance of 19, and the standing and sub-committees held 74 meetings. COMMITTEE CHAIRMEN Membership, Dr M. D. G. Salamon; Technical Programme-Metallurgy, D. A. Viljoen; Technical Programme-Mining, G. H. Grange ; Vacation School-Metallurgy, Dr P. R. Jochens; Vacation School-Mining, Dr M. D. G. Salamon; Awards, Prof. R. P. Plewman; Excursions, Dr D. I. Legge; Constitution, Rules and Policy, P. W. J. van Rensburg and Prof. R. P. Plewman; Mines and Works, P. A. von Wielligh; Education, P. W. J. van Rensburg. REPRESENTATIVES ON OTHER BODIES Associated Scientific and Technical Societies Members: V. C. Robinson and Prof. R. P. Plewman. Alternates : Dr R. E. Robinson and Dr M. D. G. Salamon. Federation of Societies of Professional Engineers Members : J. K. E. Douglas and P. W. J. van Rensburg. Alternates : Prof. R. P. Plewman and G. H. Grange. South African Council for Professional Engineers Member : R. C. J. Goode. Alternate : G. H. Grange. Engineers' Liaison Committee (Pretoria) Member: Dr J. P. Hugo. Alternate: P. W. J. van Rensburg. MEMBERSHIP Thirteen Fellows, seventeen Members, eleven Graduates, three Associate Members, eighteen Associ¬ates, twenty-six Students, and one Company Affiliate were elected during the year. Nine Fellows, four Members, and three Associates were admitted to retired membership. Eight Fellows were elected to Honorary Life Membership. Three Members and one Graduate were transferred to Fellows, nine Graduates and two Students to Members, six Students to Graduates, one Student to Associate, and one Associate to Associate Member. Six Fellows, ten Members, three Associates, and one Student resigned. A statement of membership as at June 30th 1975 and the end of the previous year is shown in the following tabulation: 30th - 30th June, - June, 1974 - 1975 Honorary Life Fellows - 9 - 15 Honorary Fellows 8 - 8 Life Fellows 170 - 170 Fellows 544 - 536 Members 512 - 523 Associate Members 10 -15 Graduates 130 - 133 Associates 194 - 210 Students 173 -175 Company Affiliates 70 - 71 1 820 - 1 851 [ ] OBITUARIES Your Council records with deep regret the death during the year of the following members: M. Barcza, Honorary Life Fellow and Past President of the Institute; J. A. Boyd, F. E. Keep and J. H. Taylor, Life Fellows; I. D. B. Corner, C. O'G. Deane, R. E. Gilmour, A. C. Hofmeyr, M. W. Howell, T. J. Robin and F. C. Steinhobel, Fellows; J. J. Frankel, Member; T. J. Higgs, Associate. FINANCE The annual accounts, which follow this report, indicate that income again exceeded expenditure by a margin of R21 410 (last year R28 524). This year's income of R71 184 showed a further increase compared with last year's figure of R55 025. Costs, however, also in¬creased, and it is calculated that, excluding non-recurrent costs, the cost of running the Institute in¬creased by R6 654 from R25 501 to R33 155 for the current year. The main increases were involved in secretarial fees, stationery and print¬ing, and in publication of the Journal. All indications are that costs will continue to rise, and we have been advised that the A.S. & T.S. will be increasing their secretarial fees by 25 per cent in the year ahead to meet their rising costs. This year's surplus was derived entirely from the revenue from sales of publications (R13 644) and a surplus from the 1974 Winter School (RIO 654). There can be no certainty that revenue from these sources can be repeated each year. Our funds are in a satisfactory position because of these worth¬while activities, but the administrat¬ion of the Institute should not de¬pend on them. Council will accord¬ingly have to give consideration in the year ahead to an upward adjust¬ment of subscriptions to meet rising costs.

Jan 10, 1975

By R. J. Mitchell

"Centrifuge modelling of earth structures is a well-proven technique for evaluating the performance of prototype structures using physical models. The applications of this technique have increased dramatically during the last decade such that even the modelling of dynamic responses in structures has been accomplished.This paper presents the first model test results used to design a mine backfill. The models were tested using a 3 m radius 30 g-tonne geotechnical centrifuge which was constructed at Queen's University specifically for model studies on mine backfill stability and subsidence. The models represent the first production blast-hole stope to be mined at Westmin Resources Ltd. 's H. ~ Mine on Vancouver Island. This paper includes photographs of:model failures in the centrifuge and correlations of model test results with analyses based on unconfined and triaxial test data.IntroductionDuring the feasibility study and development stages for the H.W. Mine, Westmin Resources Ltd. conducted a comprehensive rock mechanics and backfill engineering program. The results of these studies indicated the need for assurance of backfill stability during pillar recovery on the initial blast-hole mining block. The cemented tailings backfill had to be free standing for heights up to 25 m and the potential for surcharge loading from a weak hanging wall zone, the potential for fill block sliding down-dip and the potential for seismic loading had to be considered in the design of the fill strength. The basic questions to be answered were: what cement content is required and will the resulting backfill costs be economic relative to the proposed mining method and sequence? Figure I shows a typical cross-section through the first mining block . The up-dip stope is to be mined first and backfilled with cemented tailings . The down-dip stope would then be mined and filled. Depending on ground conditions encountered, the complete intervening pillar could be recovered and the void backfilled with uncemented tailings or it could be recovered in small sections by exposing limited back and wall areas, backfilling with waste rock and I or cemented tailings . This latter method is commonly referred to as the Avoca method"

Jan 1, 1987

By L. A. Melis, A. R. Marchbank, S. A. Webster

"Certain northern Saskatchewan uranium ores have a high content of nickel and cobalt which offer the potential for recovery as a by-product to uranium. A nickel/cobalt recovery process has been developed as a viable method of recovering a marketable concentrate from typical uranium raffinate solution.Impurities are first removed from the raffinate and the pure solution is then treated with sodium carbonate to recover a bulk nickel/cobalt carbonate precipitate for sale to a primary nickel producer. All contaminants of concern are removed to very low levels and the product is free of radioactive contamination with gamma emissions significantly below natural background. Cost estimates have shown that installation of a nickel/cobalt recovery circuit within a uranium process plant is economically feasible.The testwork that led up to the selected process is described along with recommendations for further investigations such as additional testing of hydroxide precipitation as a possible viable alternative to carbonate. The selected process is described and project economics are briefly reviewed.PROCESS TEST PROGRAMBackgroundExtensive metallurgical research has been performed over the years to develop a process for recovering uranium from the Midwest deposit in northern Saskatchewan. During the course of this research, a certain amount of information became available which suggested that recovery of nickel and cobalt from uranium raffinate could be economically feasible. It was decided to undertake a test program which would investigate methods of separating nickel and cobalt from radioactive and other metal contamination to permit production of a saleable product.Available technology suggested that three general approaches could be taken to recover nickel and cobalt. The first and simplest approach would be to selectively precipitate the impurities of concern, primarily arsenic, iron and radium, and then recover a bulk concentrate from the purified raffinate. The second approach would be to purify the raffinate and then remove cobalt from solution by solvent extraction producing pure nickel and cobalt solutions for further treatment. The third approach would be to precipitate all metals from solution and then selectively re-dissolve nickel and cobalt in ammoniac solution which would be further treated by solvent extraction for nickel recovery, leaving cobalt for further treatment."

Jan 1, 1993

By Evan Just

Throughout history mining operations have, been relatively technical in character and somewhat esoteric. In ancient times mines were places where prisoners of war or criminals were sent, to drag out short lives of hard labor, under conditions ranging from hazardous to lethal. Underground mines were damp and poorly lighted, and workers were often cramped in narrow spaces and tiresome positions. Hard rock was mined by building fires against faces and quenching with water. Combustion products from these fires and from such dim torches as were provided, plus the dampness, made the underground atmospheres quite injurious to health. During the Middle Ages, mining became less penitential and more technical. Because of the desire of sovereigns to foster production from mines, miners enjoyed special privileges as free men. Crude pumping, hoisting, and ventilation systems were introduced (Fig. 9.1). However, mining remained a relatively hardworking, hazardous occupation, separated from the lives and comprehensions of most people. With the Industrial Revolution, steam-powered pumps enabled penetration to greater depths, and the use of power-driven machinery gradually revolutionized productivity. Skill became more important than back-breaking labor. This revolution continues into the present. Mining today uses some of the largest and most complicated machinery in existence and little rock is moved by direct labor. Power drills, explosives, and boring machines penetrate and break hard rock. The modern mine, surface or underground, presents an impressive panoply of drilling, breaking, loading, and transporting equipment, facilities for power transmission, pumping, and ventilation, and expensive, complicated crushing and treatment machinery. Modern technology, machinery, and skilled workmen produce an efficiency that knows no parallel in the raw material field. Mineral substances are extracted and converted into useful forms at costs which are dwarfed by those of providing forest or agricultural products in terms of comparable weights, even though conversion of these last categories is typically much simpler. Capital investment per worker, i.e., mechanization, is greater than in nearly all other industries. Despite these features, and more than average financial risk, the mineral industries perform at modest profit. The popular concept that mines and oil fields are sources of boundless rewards is a myth, sustained by the occasional unusual episode. Before one can start actual production of minerals, he must first acquire a suitable deposit. The process of acquisition will require anything from a rather simple search to a difficult, lengthy, expensive exploration effort. After locating the desired deposit, title must be obtained by denouncement, concession, leasing, or purchase. If the deposit is solid, it can be mined in pits or underground workings. If fluid or easily fusible, it can be produced through wells. If dissolved in lake or seawater, it can be

Jan 1, 1976

By Y. G. Shiau, J. E. Burke

Several attempts have been made to account for the fact that grains in a fully recrystallized metal will coarsen on annealmg. Two fundamentally different hypotheses have been advanced, with several variations of each. One school considers that the cause of grain growth is the surface energy of the grain boundary. The theory of Jeffriesl that grain size and grain size contrast control growth is an example. The second school considers the primary cause to be a difference in the lattice energy on either side of the grain boundary. The more perfect grains are considered to grow at the expense of their less perfect neighbors, with a decrease in free energy, and a consequent increase in the stability of the system. Burgers2 presents the case for the strain or lattice imperfection theory of grain growth quite completely. The latter theory is attractive, since there is no doubt that differences in lattice energy or lattice perfection can cause grain boundary migration. A recrystallization nucleus grows for this reason as was beautifully demonstrated by van Arkel and Ploos van Amstel.³ Although it is generally stated that grain growth does not precede recrystallization, several workers4-5 have shown that small strains may induce a single crystal in an aggregate to grow, or at least may cause some grain boundary migration. The origin and nature of the imperfections that are considered to be responsible for normal grain growth have never been clearly described, but it is generally agreed that they are a consequence of the difficulty of atomic reorientation in the solid state, and that they do not seriously differ from the type of imperfection that can be introduced by mechanical deformation. An object of the present work was to determine whether the introduction of mechanical deformation would cause grain growth in a specimen which would not otherwise show it under the conditions used. It was also planned to determine the effect of such deformation on the rate of growth in a specimen which would show growth in the unstrained condition. Recently Maddigan and Blank6 have indicated that slightly strained specimens of alpha brass can undergo considerable growth prior to recrystallization if annealed at low temperatures. French7 has reported that at deformations less than 17 pet it is very difficult to detect the beginning of recrystallization in the same material. It was therefore planned to broaden this work to include a complete study of the microscopic behavior of alpha brass under condition~ of temperature, time, grain size and deformation such that recrystallization would not occur or would occur to only a Small extent. Experimental Procedure The brass was prepared by melting cathode copper and commercially pure zinc

Jan 1, 1949

By James M. Barker

Sulfur is a nonmetallic element of great physical and economic importance to the world. It is widely but sparingly distributed throughout the hydrosphere, lithosphere, and biosphere. Sulfur is the tenth most abundant element in the universe and eighth most abundant in the sun. In the earth's crust, which is mainly igneous, it ranks 14th, but is eighth or ninth in sediments (Kaplan, 1972; Stanton, 1972). It apparently is very abundant in the core of the earth, because it is a strong chalcophile, and it is fifth in abundance in stony and iron meteorites (Field, 1972) where it occurs as trolite (FeS). In ancient times sulfur was called brimstone, literally "burning stone." Today the term brimstone is used interchangeably with the term elemental sulfur. Shelton (1979) summarized most of the common definitions of terms, grades, and specifications for the sulfur industry as follows (with minor additions): Sources of Sulfur: Combined sulfur-Sulfur that occurs in nature combined with other elements. Cupriferous pyrites-Pyrite containing relatively minor amounts of copper sulfide minerals. Hydrogen sulfide-A toxic gas (H2S) occurring in natural gas and petroleum. Involuntary sulfur-Sulfur produced primarily as a result of legislative or process mandates. Native sulfur-Sulfur that occurs in nature in the elemental (uncombined) form. Nonferrous metal sulfides-Copper, lead, zinc, nickel, and molybdenum sulfides that are processed for their metal content. Organic sulfurs-Complex organic sulfur compounds occurring in petroleum, coal, oil shale, and tar sands. Pyrites-Iron sulfide minerals that include pyrite, marcasite, and pyrrhotite. Sulfate sulfurs-Sulfur in anhydrite and gypsum. Voluntary sulfur-Sulfur produced in response to market forces. Basic Sulfur Products Produced and Marketed: Acid sludge-Contaminated sulfuric acid usually returned to acid plants for reconstitution. Brimstone-Synonymous with crude sulfur. Bright sulfur-Crude sulfur free of discoloring impurities and bright yellow in color. Broken sulfur-Solid crude sulfur crushed to -8 in. Byproduct sulfuric acid--Sulfuric acid produced as a byproduct of a metallurgical or industrial process, generally relating to combined sulfur sources. Crude sulfur-Commercial nomenclature for elemental sulfur. Dark sulfur-Crude sulfur discolored by minor quantities of hydrocarbons ranging up to 0.3 % carbon content. Elemental sulfur-Processed sulfur in the elemental form produced from native sulfur or combined sulfur sources, generally with a minimum sulfur content of 99.5%. Formed sulfur-Elemental sulfur cast or pressed into particular shapes to enhance handling and to suppress dust generation and moisture retention. Frasch sulfur-Elemental sulfur produced from native sulfur sources by the Frasch mining process. Hydrogen sulfide-Associated with natural gas or petroleum and produced at refineries and coke oven plants; used to make sulfuric acid or recovered sulfur. Liquid sulfur-Synonymous with molten sulfur. Liquid sulfur dioxide-Purified sulfur dioxide compressed to the liquid phase. Molten sulfur-Crude sulfur in the molten phase.

Jan 1, 1983

By J. E. Burke, Y. G. Shiau

Several attempts have been made to account for the fact that grains in a fully recrystallized metal will coarsen on annealmg. Two fundamentally different hypotheses have been advanced, with several variations of each. One school considers that the cause of grain growth is the surface energy of the grain boundary. The theory of Jeffriesl that grain size and grain size contrast control growth is an example. The second school considers the primary cause to be a difference in the lattice energy on either side of the grain boundary. The more perfect grains are considered to grow at the expense of their less perfect neighbors, with a decrease in free energy, and a consequent increase in the stability of the system. Burgers2 presents the case for the strain or lattice imperfection theory of grain growth quite completely. The latter theory is attractive, since there is no doubt that differences in lattice energy or lattice perfection can cause grain boundary migration. A recrystallization nucleus grows for this reason as was beautifully demonstrated by van Arkel and Ploos van Amstel.³ Although it is generally stated that grain growth does not precede recrystallization, several workers4-5 have shown that small strains may induce a single crystal in an aggregate to grow, or at least may cause some grain boundary migration. The origin and nature of the imperfections that are considered to be responsible for normal grain growth have never been clearly described, but it is generally agreed that they are a consequence of the difficulty of atomic reorientation in the solid state, and that they do not seriously differ from the type of imperfection that can be introduced by mechanical deformation. An object of the present work was to determine whether the introduction of mechanical deformation would cause grain growth in a specimen which would not otherwise show it under the conditions used. It was also planned to determine the effect of such deformation on the rate of growth in a specimen which would show growth in the unstrained condition. Recently Maddigan and Blank6 have indicated that slightly strained specimens of alpha brass can undergo considerable growth prior to recrystallization if annealed at low temperatures. French7 has reported that at deformations less than 17 pet it is very difficult to detect the beginning of recrystallization in the same material. It was therefore planned to broaden this work to include a complete study of the microscopic behavior of alpha brass under condition~ of temperature, time, grain size and deformation such that recrystallization would not occur or would occur to only a Small extent. Experimental Procedure The brass was prepared by melting cathode copper and commercially pure zinc

Jan 1, 1949

Mine waste and mine reclamation are topics of major interest to the mining industry, the government and the general public. This publication and its companion volume are the proceedings of a conference held in Pittsburgh, April 19-21, 1988. There were nine sessions (50 papers) that dealt with the geochemistry, hydrology and problems of mine waste and mine water, especially acid mine drainage. These comprise Volume 1. The nine sessions (43 papers) that dealt with reclamation and restoration of disturbed lands, as well as related policy issues, are included in volume 2. Volume 2 also contains the ten papers that pertained to control of subsidence and mine fires at abandoned mines. Poster session presentations are, in general, represented by abstracts; these have been placed in the back of both volumes.

Jan 1, 1988

By F. A. Forward, V. N. Mackiw

The paper relates to the laboratory and pilot plant studies that have been carried out by Sherritt Gordon Mines Ltd., Metallurgical Research Div., in developing the ammonia pressure leach process for extracting copper, nickel, cobalt, and sulphur from high grade nickel concentrate produced from Lynn Lake ores, and describes in some detail the chemistry of the process. IT is well known'.' 2 that copper, nickel, cobalt, zinc, ferrous iron, and a number of other metals combine with ammonia in aqueous solution to form complex ions of the form [Me(NH,)x]"+. The stability and solubility of these ions depend on the concentration of the metal ion in solution, on the amount of NH, present, and on the amount and type of anions present, e.g., OH-, C0;-, NO,, C1-, SO;-. If ammonia is partially or completely removed from such solutions, for example by boiling, the soluble ammines tend to decompose and the metals precipitate as basic salts. These properties of metal ammines have found practical application in the commercial recovery of copper, nickel, and cobalt from a variety of ores. In an operation formerly conducted at Kennecott"" the mill tailing containing 0.80 pct Cu as copper carbonate was leached by percolation with an ammonia-ammonium carbonate solution to dissolve the copper as the ammine. At Calumet and Hecla0-" With a mill tailing containing about 0.4 pct Cu as metallic copper, it has been found necessary to aerate the ammonia-ammonium carbonate leach solutions between stages to oxidize the solubilized copper. At Nicarol"-" where nickel and cobalt occur as oxides and silicates which are not soluble in ammonia, the ore is heated to decompose silicates and to selectively reduce the nickel and cobalt to metal, leaving the iron as Fe,O,, and is then leached with ammonia-ammonium carbonate solution accompanied by aeration to dissolve nickel and cobalt as ammines. In each of these leaching operations, the anion present is CO, and the metals can be precipitated from the leach solution as oxide (copper) or hydroxide and carbonate (nickel and cobalt) by boil- ing off NH, and C02 both of which are recycled to treat a subsequent ore charge. The products-—oxide, hydroxide, or carbonate—can be treated by conventional smelting, calcining, or electrolytic methods to convert them to refined metals. Thus the procedures mentioned utilize the properties of the ammines to extract copper, nickel, and cobalt from nonsulphide ores and separate them from the leach solutions. These processes have the advantage that they can be carried out in closed vessels at atmospheric pressure, that the leaching solutions are specific for the desired metals, that the metals can be recovered as relatively pure compounds by the boiling operation, and that the NH, and CO, can be recycled. Also, as the leach solutions after boiling and filtration are substantially free of metals, NH,, and CO,, they can be discarded, thus facilitating the control of the water balance in the leaching circuit. When, as is the case with Sherritt Gordon concentrates, sulphides are treated with ammonia solution in the presence of oxygen, the leach solution contains SO,--, and an entirely different set of conditions is encountered. The ammine sulphates (of nickel, for example) are more soluble than the carbonates and can be only partially decomposed by boiling. The SO, and NH, in the solutions can not be recovered by boiling. Thus, despite the more favorable leaching conditions resulting from high solubility of the ammine sulphates, the recovery of metals, NH,, and SO, from the solutions must be effected by other means. Sherritt Gordon Nickel Concentrate Treatment The Ni-Cu-Co flotation concentrate produced at Lynn Lake'" contains 12 to 16 pct Ni, 1 to 2 pct Cu, 0.2 to 0.5 pct Co, 33 to 40 pct Fe, 28 to 34 pct S, 8 to 20 pct insoluble, and less than 0.02 oz per ton precious metals. The nickel is present chiefly as pentlandite, the copper as chalcopyrite, and the iron as pyrrhotite and pyrite. Most of the cobalt is thought to be present in pentlandite, although it is known that a small amount occurs as Co-Ni-pyrite.

Jan 1, 1956

By G. W. Healy

Activities of oxides in the ternary FeO-MnO-SiO system are calculated from data on the binaries, using the Gibbs -Schuhmann method. These activity data are used, together with thermodynamic relations, to calculate the contents of oxygen, silicon, and manganese in liquid iron, and the composition of the corresponding oxide phases in equilibrium with it. Excellent agreement was found between calculated and experimental metal compositions, indicating that thermodynamic methods, such as those presented, can supply useful data on slag-metal equilibria, and are therefore capable of wider application. When molten steel containing oxygen is treated with a deoxidizer, the product of the reaction is composed of the oxides of the deoxidizing elements together with more or less iron oxide. This assemblage of oxides is presumably very close to equilibrium with the melt since it is formed directly from elements dissolved in it. Therefore, it is likely that metal analyses corresponding to a given oxide phase composition are calculable with considerable precision where sufficient information is available on activities in both phases. The present study was made to test this hypothesis in the case of deoxidation by silicon and manganese. Here experimental data on the relationship among oxygen, silicon, and manganese in the metal phase are available, as are activity data for the MnO-SiO2, FeO-SiO2, and FeO-MnO binary systems. A further objective was to demonstrate in a specific example how gaps in the data may be filled by judicious interpolation, and how the Gibbs-Schuhmann method is applied to obtain activities in ternary systems. The rigorous derivation of the latter, requiring considerable facility in handling partial differential equations, tends to mask the real simplicity of the method, and repel the very engineers and experimenters who would benefit the most from its use. I) GENERAL PROCEDURE Deoxidation of steel with silicon and manganese results in the formation of two phases, metal and oxide. The number of components is four—Fe, Mn, Si, and 0. The phase rule then gives the number of degrees of freedom: If temperature and pressure are fixed, 2 deg of freedom remain. Consequently, it suffices to fix the concentration of two of the components of the system for all the concentrations to be determined and, at least in principle, calculable. The practical problem is then to discover a straightforward method of calculation with a minimum of trial and error solutions. The type of reactions to be dealt with are like the following: Si (in steel) + 2 O(in steel) = SiO2(in oxide phase) The standard free energy of this reaction is readily obtained from the literature, so that the equilibrium constant can be calculated by the expression: Since the metallurgist is concerned with percentages rather than activities, a real solution requires information that will permit activities to be converted to concentrations. This information is fairly adequate for the elements dissolved in molten steel, but is not available for the FeO-MnO-SiO2 oxide system. Therefore, the first step in this study was to find the relation between activity and concentration for the three oxides making up the system. The next step was the calculation of slag and metal compositions that are in equilibrium with one another. As shown by the phase rule, it is sufficient to assume the values of two composition variables in order to calculate the rest. But which two are picked makes a vast difference in how difficult the calculation turns out to be, so that it is necessary to make preliminary trial of several routes to find the easiest one. A convenient method is to begin with the slag, and to pick FeO concentration and that of one of the other oxides. Starting with the relation between oxygen dissolved in the liquid steel and FeO in the slag permits a good first estimate to be made of the oxygen content of the steel in equilibrium with FeO, because the iron content being fairly close to 100 pct, Fe has an activity close to unity. Using this first estimate of oxygen activity, approximate values of the manganese and silicon contents of the melt are readily calculated from the appropriate equilibrium constants. A minor correction for the depar-

Jan 1, 1963

By William A. Rhoades

INTRODUCTION Ever since miners were faced with the task of moving ore, some form of scraper has been in use. At first, men and beasts of burden supplied the power to move the scraper, and later, machines were developed for this purpose. In the early 1900s, a few mining properties used small pneumatic single-drum winches to pull loaded scrapers to a raise or ore pocket, and the empty scraper then was dragged back to the muck pile by a miner, as shown in Fig. 1. Just prior to 1920, an improvement was introduced, using two single-drum hoists. As illustrated by Fig. 2, the second hoist was used to return the empty scraper to the muck pile. However, this arrangement still re¬quired two men, one operating each hoist. The next developmental step was to eliminate the second man by locating the hoists side-by-side and using one man to control both hoists. As illustrated by Fig. 3, this involved the use of a tail rope over a sheave to pull the scraper back. The greatest progress in development and the great¬est increase in the use of slusher haulers occurred between 1920 and 1930. In 1921, the Sullivan Machinery Co. designed and built the first two-drum scraper oper¬ating on the principle illustrated by Fig. 4. It was powered by a 4.5-kW (6-hp) Turbinair(r) motor and would pull a 450-kg (1000-1b) load at 0.61 m/s (120 fpm). In 1922, this unit was shipped to the Verona Mining Co. of Caspian, MI, and it experienced immediate success in the Lake Superior iron ore district. Since the two-drum slusher was much less expensive and more efficient than hand mucking, the Lake Superior mines were saved from financial disaster when iron-ore prices fell 25% between 1923 and 1925. Immediately there¬after, a demand developed for slushers that would oper¬ate with electric power, which was considerably cheaper than compressed-air power. In 1923, the Sullivan Machinery Co. responded with the first electric-powered double-drum hoist. During subsequent years, design improvements in¬cluded separate tail-drum gearing to increase the tail¬drum speed, as welt as a number of safety features such as rope guides. One result of these improvements and their utilization by the Michigan iron mines was an in¬crease of 100% in the tons of ore per miner per day in those mines between 1924 and 1929. Since the two-drum slusher was capable only of straight-line mucking, it was not a practical machine for use in open stopes. In 1929, the Sullivan Machinery Co. introduced the first three-drum slusher. As illustrated by Fig. 5, two tail drums and one hauling drum were provided. A tail sheave could be placed at each side of the stope, and the ore then could be loaded and hauled to a central point from the entire width of the stope. During the 1930s, progressively larger slushers were demanded. By 1940, two- and three-drum units were available with motor power as high as 45 kW (60 hp), and slusher power continued to increase after 1940. Be¬tween 1951 and 1952, Joy Manufacturing Co. designed a 112-kW (150-hp) two-drum Blusher for the Climax Molydenum Co. Although there has been no demand for a slusher more powerful than this, 150- to 225-kW (200- to 300-hp) slushers are quite feasible at the pres¬ent time. During the last 30 years, many slusher improvements have been made to the operating life, operational safety, and ease of operation and maintenance. Increased tail-drum speeds have decreased overall scraping times. Rope guards, totally enclosed drums, and operator shields have reduced the hazards of injury due to wire¬rope breakage. Improvements in lubrication have made the slushers relatively maintenance-free, with long operating lives. The introduction of spring-actuated drag brakes prevented uncontrolled unreeling of dis¬engaged drums, allowing the development of practical remote-control slusher operation. Remote control now is available in a choice of all-air, all-electric, or air¬electric slushers. APPLICATIONS Quite simply, slushers are used to load and transport material (ore), generally over a short distance of from

Jan 1, 1982

By P. M. Robinson, M. B. Bever

THE heats of formation at 273°K of the compounds InBi, In2Bi, and TIBi2 have been determined by metal solution calorimetry with bismuth as solvent. The published information on the thermody-namic properties of these compounds is limited. The structure of the compound InBi (mp, 383°K) is tetragonal of the PbO (B10) type.1 The compounds In2Bi (mp, 362°K) and TIBi2 (mp of highest-melting composition, 486°K) are now believed to have structures of the NizIn (B8) type273 and not the A1B2 (C32) structures reported earlier.4, 5 The compounds In2Bi and TIBi2 have limited homogeneity ranges at room temperature, while the compound InBi has no detectable homogeneity range.' Samples of the compounds were prepared from 99.99 pet Bi (Mallinckrodt Chemical Works), 99.999 pet in (American Smelting and Refining Co.), and 99.99 pet Tl (Amend Drug and Chemical Co.) by melting the components in sealed, evacuated Vycor tubes. The compounds InBi and in2Bi were of the stoichiometric compositions. The compound TIBi2 contained 40 pet T1; this composition was chosen because at room temperature the alloy of stoichiometric composition does not lie within the homogeneity range.' The melts were held approximately 50°C above the liquidus for 8 hr and then quenched into iced brine. The samples were homogenized for 48 hr at temperatures 20°C below the temperature of complete solidification. Metallographic examination of sections taken from the center and the ends of the ingots did not reveal second phases or segregation . The heats of formation were determined as the difference in the heat effects on solution of a compound and of a mechanical mixture of its components added from the reference temperature of 273°K to liquid bismuth at 623°K. The details of the calori-metric procedure and method of calculation have been described elsewhere? The calorimeter was calibrated by adding bismuth at 273°K to the bismuth bath at 623°K. The calculated values of the heats of formation of the compounds, listed in Table I, are based on a value of 4.96 keal per g-atom for the difference between the heat contents of bismuth at 273" and 623oK7 No published values are available for the heats of formation of the compounds InBi and In2Bi. Hultgren et a1.7 have calculated a value of -0.50 i 0.10 keal per g-atom for the heat of formation at 423°K of the compound TIBi2 containing 40 at. pet T1 from heat-content measurements in the range from 398" to 700°K and the heats of formation of the liquid alloy. The difference between this value and the value of -0.66 * 0.01 keal per g-atom at 273°K is too large to be attributed to a difference between the heat capacities of the compound and the components over the temperature range 273o to 423oK7 However, the direct determination of the heat of formation by a calorimetric method should give a more accurate value. The heats of formation at 273°K of the compounds InBi and In2Bi lie on a straight line when plotted as a function of composition, Fig. 1. The compound In2Bi, therefore, appears to be barely stable with respect to its neighboring phases. In order for the free energy vs composition curve to be concave towards the composition axis, the entropy change on formation of In2Bi must be more positive than that on formation of InBi. As the compounds are ordered,2, 3, 8 there is no configurational entropy change on formation. The difference between the entropy changes on formation of the two compounds, therefore, is probably associated with the vibrational entropies. In view of the low heats of formation, the changes in vibrational entropy, due to changes in bond strength on formation of the two compounds, are likely to be small. Owing to the volume contractions on formation of the two compounds,5 the vibrational entropies probably decrease slightly but the decrease of the vibrational entropy of InBi is expected to be larger than that of In2Bi.

Jan 1, 1965

By H. J. Ramey

Conventional calculation of total system isothermal compressibility for a system containing a free gas phase involves, among other things, evaluation of the change of oil and gas formation volume factors and the gas in solution with pressure. Preferably, this information should be obtained from laboratory measurements made with particular oils and gases. Often, experimental measurements are not available. In this case, it is necessary to obtain pressure-volume-temperature relationships from general correlations such as those of Standing' for California oils. In order to speed estimates of compressibility, generalized plots have been prepared of the change of both oil formation volume factors and gas in solution, with pressure from Standing's correlations. A generalized plot for estimating the change in the two-phase (oil and gas) formation volume factor with pressure is also presented. Usually, the effect of gas dissolved in reservoir water upon the total system compressibility is neglected for gas saturated systems, due to the low solubility of gas in water. Results of this study indicate that the increase in total system compressibility caused by solution of gas in water is often as large as the compressibility of wafer, and can be magnitudes larger for low pressure systems. Generalized results for estimating the change of gas in solution in water with pressure are presented in tabular and graphical form. INTRODUCTION During the past decade, pressure build-up and drawdown techniques have gained an important place in reservoir engineering. Build-up and drawdown analyses are only two special applications of the broad field of transient fluid-flow theory. All solutions of transient fluid-flow problems contain a parameter called the total system isothermal compressibility. This property of fluids and porous rock is a measure of the change in volume of the fluid content of porous rock with a change in pressure, and it may vary considerably with pressure. Evaluation of total system isothermal compressibility is not difficult, but it is tedious and time-consuming. Often compressibilities are estimated roughly, or transient flow methods are neglected completely. The benefits of using accurate system compressibility in properly-executed build-up or drawdown analyses are: 1. Better planning of pressure build-ups may be achieved to avoid unnecessary loss of revenue due to excessively long shut-in periods, or to shut-in periods too short to yield useable data. 2. Better and more reliable estimates of static formation pressures for reserves estimates and rate performance estimates. 3. Reliable information for evaluation of well completion effectiveness, and planning and interpretation of well stimulation efforts. The purpose of this paper is to clarify the nature of the total system isothermal compressibility, and to present useful methods for estimation of compressibility, particularly for systems containing a gas phase. DEVELOPMENT Numerous publications have presented solutions to transient single-phase flow of slightly compressible fluids, stressing pressure build-up applications. In transient flow, a compressibility* term arises to permit volume content of fluids in porous rock to change as pressure changes. The basic nature of the compressibility term is usually taken for granted. Problems arise in practical applications of transient fluid theory because most published works consider only one flowing fluid—in an ideal porous system containing only one fluid. In 1956, Perrine2 presented an intuitive extension of single-phase flow pressure build-up methods to multiphase flow conditions. Later, Martin- established conditions under which Perrine's multiphase build-up method had a theoretical foundation. Perrine has shown that improper use of single-phase build-up analysis in certain multiphase flow situations can lead to gross errors in estimated static formation pressure, permeability and well condition. It is likely that, much pressure build-up data for oil wells should be analyzed on the basis of multiphase flow. For both single-phase and multiphase build-up analysis, the isothermal compressibility term in dimensionless time groups often should be interpreted as the total system compressibility. All real reservoirs contain one or more compressible fluid phases. In addition, rock compressibility can contribute in an important way to the total system compressibility. The proper total system compressibility expression may contain terms for compressibility of oil, gas, water, reservoir rock and terms for the change of solubility of gas in liquid phases.

Jan 1, 1965

By H. A. Hoffman

Competition from an all-flotation plant, with demonstrated economies and efficiencies, plus a change in smelting contract and introduction of improved cyclones lead to conversion from gravity-flotation. Detailed descriptions are given of equipment installed and procedures used at St. Joseph Lead's Federal mill. Future plans include further quality control by instrumentation in all aspects of the mill operation. Also planned are improvements in materials handling systems. Competitive conditions will continue to dictate improvements and changes in the mill flowsheet. The advent of all-flotation mills in the Lead Belt was introduced by the Indian Creek mill in late 1953. This modern and efficient plant then became a pattern for the other mills in this area to re-evaluate their circuits in an effort to develop flowsheets that would improve operating conditions and metallurgy. The Indian Creek mill demonstrated that all-flotation would require considerably less operating and maintenance labor than the combination of tabling and flotation that was common in the Lead Belt at that time. Two significant changes occurred in recent years to allow all-flotation to be seriously considered in other Lead Belt mills. One was a change in the smelting contract which did not require gravity concentrate. Another was the development of cyclones which provided classification of the flotation feed in a very small space. Since the Federal mill was the largest concentrating plant in the Lead Belt it was felt that the greatest savings could be made by investigating the all-flotation possibilities at this mill. Interest was stimulated by the milling and ore dressing Depts. to determine if this mill would be converted without undue cost, provided the metallurgy could be improved. Accordingly, laboratory tests were initiated to learn what metallurgical benefit could be derived. Numerous tests were run which indicated that grinding to all-flotation would improve the tailing by as much as 0.02 pct Pb. This was quite significant when multiplied by the tonnage of ore treated. Projecting the added cost of power for extra grinding and flotation, and the additional flotation reagents required, plus additional new equipment that would have to be purchased, it would still add up to a considerable saving. The all-flotation mill would reduce man power by some 30 pct, and make a metallurgical improvement. Operating costs could be reduced bv 2$ per ton. The metallurgical improvement would amount to 4$ per ton, for a total of 6$ per ton of ore milled. An estimate of the cost of the conversion was set at $250,000. With the savings as estimated this could be paid off in about two years. On paper it therefore seemed attractive enough to justify a mill test. MILL TESTING One section of the Federal mill was made available for use as a separate test circuit. Cyclones and density controllers were borrowed from the Viburnum and Indian Creek mills. Denver flotation cells were obtained from the Desloge mill that was then shut down. Two 10-cell groups of Fagergren flotation machines, consisting of eight roughers and two cleaners in each bank, were segregated from the remainder of the plant. The 9x12-ft rod mill was continued as a primary grinding mill. The two 6%x12-ft mills on this section were converted from rods to balls, and the speed increased to 22.0 rpm. Cyclones were installed to close the circuit of these ball mills. The ground pulp from each of the ball mills was fed separately to its own bank of flotation cells so that two completely separated test circuits could be run in parallel. This test circuit operated on a three-shift basis from Dec. 22, 1959 to Mar. 21, 1960. The first few weeks were occupied in developing conditions for proper metallurgy and trouble-free operations. Results were rather erratic but as the ore dressing laboratory and the mill operators became more familiar with conditions they were able to obtain expected results, which could be duplicated day after day. The last five weeks of testing indicated the best results and are tabulated in Table I. During the first two weeks a Denver unit cell was used on No. 1 flotation circuit. Even though it recovered almost one half of

Jan 1, 1962

By B. L. Averbach

Recovery and primary recrystalliza-tion in cold worked metals are usually considered as two competing processes. Some of the effects which usually accompany recovery are: alleviation of stress corrosion tendencies, changes in thermal emf,1 damping capacity,2 electrical resistivity,2 and magnetic properties,3 and only minor changes in hardness or the related strength properties. During primary recrystalliza-tion new unstrained grains are formed at the expense of the strained matrix. These new grains eventually become visible metallographically, and nucle-ation and growth kinetics have been indicated for this process.4,5 Frequent attempts have been made to study the cold-working phenomenon by observations on the line broadening by X ray diffraction patterns. Relatively few measurements of line intensities have been made, although Brind-ley and his collaborators, 6,7,8 by means of film techniques, compared the intensities of cold worked Cu, Ni, and Rh patterns with those from chemically precipitated powders. These precipitated powders were presumed to be strain free, and it was found that the intensities for the cold-worked materials progressively decreased as the Bragg angle increased except for the first line, where there was an increase due to reduction in extinction. This was interpreted as a randomness in atomic position induced by cold work. Such randomness is similar to that caused by thermal agitation and has been described as "frozen heat" displacement of 0.08-0.10 A from the mean atomic position. In a recent study9 on the effect of cold work in metals on their powder pattern intensities, the changes in integrated intensity for heavily cold worked alpha brass were observed as a function of the annealing temperature. These measurements were made with a manually operated Geiger-counter spectrometer using CuKa radiation monochromated with a rock salt crystal. Intensity measurements were made with a scaling meter over small intervals of angle, and the equipment was so arranged that the diffracted and incident beams made equal angles with the specimen. Intensities could be compared directly by simply interchanging specimens, and comparisons from day to day were made with a standard whose line intensities did not change on aging. It was shown that a cold worked alpha brass standard was stable for at least a year. Table 1 indicates the results of the integrated intensity measurements on a 70 Cu-30 Zn brass. In the sample preparation, a brass plate was first cold rolled 50 pct and then filed, screened to —325 mesh, compacted into briquettes at a pressure of 60,000 psi and finally annealed for one hour at various temperatures up to 400°C. The briquetting pressure did not seem to influence the integrated intensities, and most of the cold work was introduced by the filing. Although this method of cold work is not quantitative, it was used to obtain random orientation (and thus uniform diffraction lines) in order to make accurate measurements of integrated intensity. Back reflection patterns were taken in each case to check the uniformity of the lines, and from the observed line broadening it was apparent that this type of plastic deformation was quite severe. Care was taken to traverse the entire background of the pattern and to assign to each peak the total intensity above this background. The bases of the diffraction lines were quite broad and spread out over several degrees, even for the narrow peaks. The theoretical intensities were calculated to include a temperature correction, a dispersion correction, and a Lorenz- polarization factor corrected for the crystal monochromated beam. In Table 1 it was necessary to match the calculated and observed values at only one point, and the rest of the experimental values were converted directly to this arbitrary scale. The integrated intensities in Table 1 are listed in arbitrary units, and the accuracy was sufficient to reproduce any of the measured line intensities to within + 1.5 units. It is evident that the percentage error on the strongest line (111) was quite low. The calculated values and the observed intensities for the cold worked material matched reasonably well. As the annealing temperature was raised, however, the intensity of the strongest reflections, particularly the (lll), decreased measurably. Since the background intensities of all of these patterns were identical, such behavior could be interpreted as a primary

Jan 1, 1950

By F. V. Lenel, G. S. Ansell, J. A. Dromsky

The growth of aluminum oxide particles in a nickel matrix was studied eve?. the temperature vange of 2140° to 2470°F. The instability of the dispersed alumina was shown to be independent of the crystal structure of the alumina. The activation energy for the growth of the dispersed alumina was found to be 84.7 1 2.0 kcal. The particle radius increased as a function of time. These results indicate that the growth is not diffusion controlled. It is believed that the rate controlling mechanism is the dissolution of the aluminum and oxygen atoms into the nickel lattice. THE strength properties of alloys which consist of a finely dispersed second phase in a metallic matrix depend upon the spacing between the second phase particles. It is therefore desirable to achieve very fine dispersions in these alloys. Furthermore, to retain the properties these very fine dispersions must be stable during fabrication and service of the alloys. The best known of the dispersion strengthened materials, the SAP type alloys, which consist of a dispersion of aluminurn oxide in aluminum, have exceptionally good stability up to the melting point of aluminum. There is evidence, however, that other dispersion strengthened alloys, even those consisting of refractory oxides in a metal matrix, may be less stable. This investigation is concerned with the stability of Ni-Al2O3 alloys in the temperature range in which these alloys are usually fabricated. The mechanical properties of Ni-Al2O3 alloys at elevated temperatures have been previously investigated by Crelnens and rant,' and Gregory and Goetzel.2 The behavior of these alloys in stress rupture tests appears to indicate that at temperatures below 1800°F they are highly stable. There is some doubt, however, as to their stability at the higher temperatures used during the conventional fabrication. Cremens and Grant, in preparing their test alloys, cousolidated, by powder metallurgical techniques, nickel powders as fine as 0.13 µ diam and alumina powders as fine as 0.018 µ. Metallo- graphic examination of the alloys following fabrication revealed that none had interparticle spacings of less than 2 µ. Considering the size of the original component powder particles, it is likely that the dispersions coarsened during fabrication. Gregory and Goetzel, in their studies of extruded alloys of 80 pct Ni—-20 pct Cr matrixes with nonmetallic dispersion, observed a definite coarsening of the alumina dispersions in alloys sintered at 2280°F as cantrasted to those sintered at 2000oF. Similar observations on the spheroidization and growth of thoria particles finely dispersed in a nickel matrix were made by D. K. Worn and S. F. Marton.3 As a result of such coarsening, much of the effort expended in the preparation of very fine powder mixtures would be lost. The mechanical properties of the alloys which had experienced coarsening would be expected to be poorer than if the original dispersions had been retained. EXPERIMENTAL PROCEDURE Ni-Al2O3 alloys were produced from powder prepared by a coprecipitation technique. Aluminum hydroxide and nickel hydroxide were coprecipitated from chloride solutions of the metals. The mixed hydroxides were calcined to form metal oxides and the nickel oxide in the mixture was selectively reduced to nickel by treating it in hydrogen. Specimens were compacted from the resultant powder which consisted of a fine, uniform mixture of aluminum oxide and nickel particles. The compacts were sintered by resistance hot pressing4, a densification technique which requires exposure times of the order of only a second or less at elevated temperatures. A conventional sintering process was not used, since the temperature required for densification would have to be in the region in which the stability of the dispersion was to be studied. A series of hot pressed specimens were treated in hydrogen at temperatures from 2140o to 2470°F (1171o to 1355oC, for times up to 120 hr. Changes in the microstructures were studied by electron microscopy using the two-stage preshadowed carbon replica method.5 In performing a lineal analysis on a series of micrographs from each specimen it was found more convenient to determine the mean free path between alumina particles rather than particle radii as the parameter of growth. Although these quantities are directly proportional for only spherical particles, the alumina particles in these alloys

Jan 1, 1962