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By R. D. Lee

A simplification of the method of Hurst and McCarty for conducting potentiometric model studies by the single probe method is presented along with experimentally determined invasion patterns for certain idealized flow problems. The analytical solution for one class of these problems is given. Finally, a general description is given of a newly developed instrument which permits direct mapping of flow lines and determination of transit times in potentiometric-model studies. Introduction The object of this paper is to present: I. A simplification of the method of Hurst and McCarty for conducting poten-tiometric-model studies of oil and gas reservoirs by the single probe method. 2. Results of a series of studies of certain idealized flow problems and the general conclusions to be drawn therefrom. 3. A description of a new instrument, the Chronocartograph, which greatly reduces the labor and time required for conducting potentiometric-model studies. Certain general conclusions may be drawn as results of the investigation of the idealized flow problems. They are: I. Injection and extraction areas should be separated by as great a distance as conditions permit since, in general, the recovery prior to first breakthrough tends to vary as the square of this distance. 2. Little advantage is to be gained by use of more than eight injection wells or groups of injection wells for the case of circular productive limits. 3. Elongated shapes of productive limits are best exploited by injection on the extended major axis only, with a line of extraction wells lying on the major axis. 4. The use of peripheral injection wells for elongated shapes is permissible, if necessary, but requires extension of the line of extraction wells. The exploitation of an oil or gas field is effected either by the expansion of the gas and oil, or by their displacement by another fluid. Both methods may be used simultaneously. When the displacement of the oil or gas is the controlling factor there arises the problem of mapping the progress of the boundary between the fluid in place and the displacing fluid. This problem is of particular interest in the operation of a cycling project in a gas-condensate field, where the wet gas is produced from one or more wells, commonly called "extraction wells.'' This wet gas is taken into a processing plant where the condensate is removed. The remaining "dry" gas is injected back into the field through one or more wells, called "injection wells," both to conserve the gas for future use and also to maintain the pressure in the field. In an operation of this type it is essential to anticipate the manner in which the dry gas will spread through the field, because the ultimate recovery of the wet gas depends

Jan 1, 1948

By Raymond B. Ladoo

Abrasives include the substances, natural or artificial, that are used to grind, polish, abrade, scour, clean or otherwise remove solid material, usually by rubbing action but also by impact (sandblasting, for example). They do not include abrasive tools-for instance, lathe tools and files-or polishing agents such as waxes, which act by filling pores. Detergents and cleaners whose action is chemical rather than physical are omitted although some chemical-action polishes and cleaners may also contain solid abrasives; for example, many automobile and metal polishes. General Considerations The most important physical properties of materials that qualify them for use as abrasives are hardness, toughness (or brittleness), grain shape and size, character of fracture or cleavage, purity or uniformity. For making bonded grain abrasives such as grinding wheels, additional important factors are stability under high heat and bonding characteristics of grain surfaces. The economic factors of cost and availability are always important. No one single property is paramount for any use. For some uses extreme hardness and toughness are needed, as in diamonds for drill bits; for others, the factors of greatest importance are hardness and ability to break down slowly under use, to develop fresh cutting edges when grains become worn-for example, in garnet for sandpaper, neither highly cleavable or friable grains nor extremely tough grains are wanted. For still other uses, great hardness is objectionable; for example, abrasives for dentifrices and for glass-cleaning soaps. For the most efficient use in the more critical applications, the different types of abrasives are rarely completely interchangeable; thus, while crushed quartz and garnet are both used in sandpaper, the papers are not at all interchangeable in their use applications. In the last analysis, the choice of a high-grade abrasive depends upon the quality and quantity of work done by the abrasive per unit of cost. Initial cost of an artificial abrasive. may be much greater than that of a natural abrasive but the artificial abrasive may do so much better work than the natural one, and do it so much faster, that the ultimate cost will be less. It is on this basis that artificial abrasives have largely replaced natural abrasives for grinding metal. Classification Abrasives may be divided into two general classes, natural and manufactured. The former includes all rocks and minerals used for abrasive purposes without chemical or physical change other than crushing, shaping or bonding into suitable forms. Manufactured or artificial abrasives are made either by heat or chemical action from metals or mineral raw materials. On page 2 is a list of the most important abrasives, classified as to inherent types and as to forms in which they are used industrially. For most types of use there are manufactured products that can be substituted for the natural products, usually at higher initial

Jan 1, 1960

A. H. Mokken: I am pleased to have been given this opportunity to make a contribution to Dr Muller's paper tonight. The reason for this is that, at one stage in our careers, we were associates in the same undertaking. Dr Muller, then fresh from University, with a degree in pure science, had just stepped onto the first rung of the ladder, which, it was then thought, would lead him to a career in gold extractive metallurgy. However, endowed with an enquiring mind and conscious of a lack of fundamental training in general metallurgy and engineering, he felt a need for further academic study. To meet this need and, more importantly, to meet the necessary finances, he found his opportunity in steel. Armed with a bursary, he bade farewell to gold and proceeded overseas, to the University of Sheffield, to train as a steel metallurgist. The outcome of these academic efforts, which were followed by assignments in the steel industry and a further period at Sheffield, is the man we have listened to tonight-a highly qualified metallurgist who has displayed a sound knowledge of his subject. In choosing Sheffield, Dr Muller became associated with a steelmaking centre of world renown, a centre usually credited with the first systematic production of alloy steels, as far back as the 18th century. Since that time, great advances have been made in the production of alloy steels and this is especially so in the last decade or two, when major developments in civil, mechanical, electrical, aeronautical and nuclear engineering have been made possible by the development of steels with improved properties. In spite of spectacular advances in the technology of non-ferrous alloys, plastics and other materials of construction, steel has maintained its role as a pre-eminent material for engineering use. With the gradual accumulation of data on the properties of steels, and the use of thin film electron microscopy, to study the behaviour and characteristics of such phenomena as dislocations in metals and other microstructural features, the physical metallurgist appears to be approaching the stage of an exact understanding of such phenomena as strength, ductility and brittleness-a knowledge which could lead to close control of such properties and, therefore, to the attainment of the highest goals. An interesting example, illustrating the use of fundamental principles, based on physico-metallurgical research, is the development of the maraging steels developed by Bieber at the International Nickel Company. These steels have met the extreme technological requirements of the space age by providing the material for the cases of large rockets in which qualities, such as high tensile strength, toughness, workability and weldability are most important. Attractive as they might appear to be in considerations of savings of weight, cost of erection, transport of materials and foundations, the use of high strength steels has been accompanied by special problems such as brittle fracture, hydrogen embrittlement, notch-toughness and fatigue. It has been found that high strength steels, which performed acceptably in conventional tension tests, were found to undergo failure, in a brittle manner, in service. Hydrogen embrittlement has caused spectacular failures at a fraction of the normal ultimate tensile strength, and a lack of correlation between fatigue and tensile strengths has diminished the advantages to be obtained from the use of high strength steel in some applications. A new approach to the selection of materials for engineering design has resulted from a consideration of these phenomena in which strength, as such, is no longer as significant as it was previously. Parallel with the development of high strength steel has been the need for suitable techniques for joining component parts and here welding has played an

By P. R. Jochens, D. D. Howat, R. B. Atmore

INTRODUCTION The Miller chlorination process has assumed a preeminent position in the refining of gold bullion, a position it has maintained for over half a century. In the early sixties considerable interest was aroused by the idea of producing a consistently high grade bullion at the mine smelthouses themselves. However, as the use of chlorine in industrial plants is associated with considerable hazards, oxygen was considered a natural alternative, apart from bing less expensive than chlorine. Partial refining at the mine smelthouses would considerably decrease the requirements made on Rand Refinery Limited as well as indicating the possibility of reducing final refining costs. An added factor would be the purer silver chloride obtainable, after prior removal of the base metals by oxygen injection, which would facilitate the production of high-purity silver. The free energies of formation of the oxides of the metals;- silver, copper, lead, zinc, iron and bismuth indicate that, with the exception of silver, these metals should be capable of removal as oxides by oxygen injection. Rose1 had shown that during injection of gold bullion, considerable loss of silver to the boraxsilver slag occurred and, furthermore, that copper removal was not efficient and oxide attack on the refractories was severe. Plant test work2 had confirmed the difficulty of copper removal, but had shown that zinc and lead were almost completely removed. The difficulty of copper removal by oxygen injection warranted further investigation. Also, the high decomposition pressure of silver oxide suggested that by suitable control of the slag composition it might be possible to reduce to very small proportions the silver carried into the slag as oxide. The oxidation of copper by oxygen injection and subsequent dissolution of the oxide in a slag may occur according to the following reactions; Reactions 4 and 5 were considered because of the relatively high solubility of oxygen in molten silver and silver alloys. Thermodynamic data indicate that there is little possibility of any reaction involving the formation of CuO occurring at temperatures above 1 000 °C. To ensure that the operative reactions 1 and 4 take place to the maximum extent, the following factors He significant. (a) an increase in the activity of the copper in the bullion, (b) an increase in the partial pressure of oxygen in the system, (c) an increase in the activity of the oxygen in solution in the metal, (d) a decrease in the activity of cuprous oxide in the slag. From practical considerations, the operative variable most easily susceptible to control is the composition of the slag. SOLUBILITY OF COPPER OXIDES IN BOROSILICATE SLAGS Very scanty information exists on systems containing copper oxides but the indications are that slags containing considerable amounts of boric oxide would possibly prove to be the best solvents for cuprous and cupric oxides. This is attributed to the fact that the activities of copper oxides are much lower in boric oxide slags than in slags in which silica is the main network former. The number of possible slags containing boric oxide was limited by consideration of liquidus temperature, viscosity, corrosive action on refractories, volatilization, and ultimately cost (for industrial application). Slags in the systems soda-boric oxide-silica and lime-boric oxide-silica were selected paying due attention to the above limitations. Additions of 5, 10 and 15 per cent cupric oxide were made to the finely ground, premelted slags. These mixtures were then reground and 2g quantities held in re crystallized alumina crucibles at temperatures of 1150°C and 1 250°C respectively for 30 minutes. The crucibles were removed from the furnace, rapidly cooled, cut in half longitudinally, and a thin section taken from one half was subjected to microscopic examination.

The visit which took place on the 18th February, 1972 was a departure in that the places visited had no direct connection with the work in which members of the Institute are normally engaged. It was refreshing and stimulating to see important and involved operations normally outside ones own trend of life and to have experts to speak about technical, financial and matters of general interest concerning their work, not forgetting their troubles and problems and how they overcame them. Carlton Centre The members of the Institute were received by Mr D. Appleton, Public Relations Officer of the Carlton Centre Limited, who introduced Mr L. R. M. Fee of W. Rhodes Harrison, Architect in charge of the project; Mr W. C. E. Skilton of Murray and Roberts, the Engineer in charge of the construction of the complex and Mr A. Home the Senior Operating Engineer of Carlton Centre Limited. Each of these gentlemen addressed the members giving short rundowns on the project with special reference to their particular sphere of the undertaking. A variety of particularly interesting statistics relating to the planning construction and the ultimate operation and maintenance of the complex was given. Mining engineers present had an opportunity to compare the problems encountered by them associated with depth to problems encountered by the civil engineer in the construction of a building rising to such an enormous height. To some of the members a sense of similarity of the labour problems encountered must have been recognised. After tea the visitors were divided into groups, each under the guidance of an official, and then visited the highest floor accessible and thereafter the 19th floor where the internal arrangements for airconditioning, lighting, plumbing, power supply and communication arrangements were explained. Thereafter a visit to one of the seven basements which houses all machinery required to serve this enormous complex enabled the visitors to see the standby power arrangements as well as the refrigeration plant. The visit finished in time to proceed to the Crest Hotel in Hillbrow for lunch. To our hosts for the visit to the Carlton Complex a special vote of thanks is recorded. Strydom Tower In the afternoon the party proceeded to the Strydom Tower where Mr Knight from the Public Works Department who was the Engineer in charge of the construction of the tower gave details on the construction and the extraordinary methods which had to be adopted to achieve the desired objectives and to overcome known as well as unforeseen difficulties. The comparatively short time taken to complete the project and the good safety record appeared to impress the visitors. The final phase of the visit was taken care of by Mr Bothma of Telecommunications Department of the Post Office, who gave an extremely interesting explanation of the telecommunication organization of the Post Office with particular reference to the part the Hillbrow Tower plays in the South African telecommunication system. Both gentlemen answered many questions willingly and interestingly. Following the explanatory talks the visitors were shown the technical equipment housed in the two top levels of the tower. Short explanatory talks gave members an insight into the workings of one of the most important aspects of modern life. Even to the amateur photographer opportunities existed to view and photograph the city from the highest available observation point. We are indebted to Mr Gouws, the Regional Director of the Post Office for granting permission to visit sections of the tower normally not accessible to the general public and to our hosts for the manner in which we were received and entertained on the explanation of the many interesting features of this important installation. In conclusion, the programme for the day can be classified as interesting, of exceptional educational value, and an opportunity to see something of the engineering skills put into two vast and ambitious undertakings and the results achieved.

INTRODUCTION Mineral explorationists range throughout the world looking for mineral deposits which can subsequently be made into mines. Mines are not found! Mines are made, usually at great cost and not often without significant risk. The process of making a mineral deposit into a mine involves a great deal more than a complete appraisal of the deposit. The making of a mine demands detailed feasibility studies of many factors, any one of which, if shown to be negative, could prevent the deposit from becoming a successful mine. Total feasibility analysis involves at least three major fields of study: (1) economic analysis, (2) financial analysis, and (3) political and environmental analysis. Economic analysis is essential for proper decision making at many stages in the evaluation of a mineral deposit. It is the yardstick by which the proposed mining project and alter- native investment opportunities are measured. Economic analysis is concerned with costs and potential profits and can be applied at various stages in the evaluation of a mineral deposit to determine if the project merits the additional funds necessary to bring about each succeeding stage. The nearer any deposit approaches to becoming a mine, the more carefully the economic analysis should be made. Financial analysis has reference to how, where, and at what cost the investment funds can be obtained to finance the proposed mine project. Political and environmental analysis has reference to the many intangible factors that can affect the making of a successful mine. These factors loom larger today than ever before, due to the profusion of government regulations and various environmental constraints now imposed upon the mineral industry both by law and by the weight of public opinion. Ultimately, many of these intangible factors can be resolved back into the economic analysis as an added cost to mine development, but more and more often they have become insurmountable obstacles to any development of certain deposits. The role of financial analysis and the analysis of intangible factors must never be underestimated when making a feasibility study upon which to base investment decisions; however, the emphasis of this text will be upon economic factors. THE PARAMETERS OF MINERAL ECONOMIC ANALYSIS The two major elements of economic analysis are: 1) The potential earnings or annual generated cash flow of the project. 2) The investment costs necessary to realize such earnings. If the difference between the two elements is large enough, i.e., if the return on investment from the cash flow is high enough to attract investors, the project can be said to be financially feasible. The mineral economic analysis must take into consideration many parameters, some of which are known or knowable within certain limits, and others of which are unknown or unpredictable within certain limits and for which estimates must be made. Because both known and estimated parameters enter into the same analytical computations, it is important for the analyst to realize the nature of each when considering the results of an analysis. Some parameters such as the grade of mining block, although estimated, are said to be known within mathematically defined limits. Other parameters, such as the future price for minerals produced, etc., can only be estimated or "guestimated" within reasonable limits for which no precision can be assigned. Known or Knowable Mineral Economic Parameters Known or knowable parameters are: 1) Tonnage and grade of valuable minerals for the total mineral body and for individual mining blocks. 2) Metallurgical recovery of valuable mineral. 3) Minimum operating life of mineral de- posit at any specified production rate. 4) Royalty schedule, property payments, etc. 5) Sales-purchasing agreements, smelter schedules, marketing contracts, etc.

Jan 1, 1980

By C. G. Dunn

The measurement of interfacial teusions or grain boundary energies in metals is an important metallurgical problem, especially since it bears on growth and nucleation processes. Statistical methods of measuring equilibrium grain boundary angles, which relate interfacial tensions, have been used by some investigators1'2 but more direct methods would be preferred. A direct way, based on a simple extension of a successful method of growing single crystals of silicon ferrite to predetermined orientations in flat specimens,3 is to produce three-grain specimens in such a way that the equilibrium common grain boundary will be perpendicular to the surface of the specimen. The angles to be measured then appear as the grain boundary angles in the surface of the specimen. The method of producing a single crystal specimen with a predetermined orientation is basically the same as that employed by Yoshida and Fuji-wara4 in their work on aluminum wires. The specimen, prior to any single crystal transformation, must have a matrix which will support the growth of a crystal of the desired orientation. Growth may occur through exaggerated grain growth or, if the matrix is strained a critical amount. by normal recrystallization. In either case the matrix must have stability at the temperature used to effect the transformation, this stability appearing as a long induction period for exaggerated grain growth or for the formation of recrystallization nuclei. Additional control is gained by using a high temperature gradient through which the specimen is moved at a suitable rate. To obtain the desired orientation, the specimen is fed a short way into the furnace producing one or more crystals in the hot end. After the specimen is removed from the furnace, the orientation of a crystal is determined, so that this crystal may be reoriented by properly deforming a narrow piece of the matrix between the end crystal and the rest of the specimen. This part of the specimen in the case of silicon ferrite is preferably held at red heat during the reorienting process. Fig 1 shows a specimen which is ready to be transformed into a single crystal through growth of a reoriented "seed" crystal. When the method just described is applied to the production of a three-grain specimen two crystals are grown first side by side in one end, the specimen is then reversed and the third grain grown from the opposite end. A suitable group of grains each of different orientation is one where all three grains have the same crystallo-graphic plane in the plane of the specimen. Fig 2 shows a photograph of a three-grain group prepared as described. The notches are introduced in the open ends of the grain boundaries to anchor them during the final annealing operations which ultimately should bring the grain boundaries to the lowest energy configuration. Two-grain groups with different crystallographic planes in the plane of the specimen can be similarly prepared and treated. If the two grains have different surface (gas to metal) energies per unit area, the equilibrium condition leads to a curved grain boundary.* * This feature of the problem was pointed out by J. c. Fisher. References 1. Cyril Stanley Smith: Grains. Phases and Interfaces: An Interpretation of Microstructure. Trans. AIME 175, 15. Met. Tech. TP 2387, June 1948. 2. D. Harker and E. Parker: Grain Shape and Grain Growth. Trans. A.S.M. (194,5) 34, 156-195. 3. C. G. Dunn, A. Seddon, and R. Wylie: Unpublished Work, 1946-1947. 4. Takeo Fujiwara: A Method of Producing A Long Single-Crystal Wire of Aluminum with any Desired Crystallographic Axis. Jnl. of Sci. Horoshima Univ. A, (1939) 9, No. 3, 227.

Jan 1, 1950

By Whitman E. Brown, Louis J. Erck

L. A. ROE*—This paper is one of great value to the iron ore industry. The Humphreys spiral is a relatively new tool and gives promise of being quite useful in solving certain problems of iron ore beneficiation. Spirals have been tested on a martite ore at the Benson mine of Jones and Laughlin Steel Corp. in northern New York State. Our New York ore is considerably different, physically and mineralogically, than the one mentioned in this paper, and contains only 25 pct iron. This ore can be processed on spirals to give a concentrate containing 62 pct iron with an 85 pct recovery. On our particular ore we found operating difficulties when the spiral feed was coarser than 14 mesh. These were chiefly due to excessive "build-up" of locked middlings in the spiral circuit. In extreme cases these middling particles would accumulate to such an extent that the plant had to be shut down and the spiral surge tanks cleaned out. It is interesting to note that there exists a close relationship between the results of tabling a given iron ore and concentration of this same ore on Humphreys spirals. The size range of the ore must, of course, be within those limits acceptable to spiral concentration. Comparative tests on several of our mar-tite ores showed tabling results to be the same as spiral results. The authors make no mention of the use of a tailing stream splitter (now available from the spiral manufacturer) which is a useful tool in studying iron losses in the tailings stream. 011 our particular martite ore we found a considerable accumulation of fine-sized iron ore particles in the outside portion of the tailings stream. This fraction may be amenable to further treatment. E. H. ROSE*—The authors have concluded an interesting piece of work and this paper is an excellent factual account of a rapid and somewhat unusual transi-;ion in practice in the plant described. Perhaps it was modesty on their part which caused them so casually to limit to one sentence the fact that "several other methods of concentration on the fine ores representative of the Hill Trumbull group . . . failed to produce consistently an acceptable grade and recovery of finished product." The fact is that they were confronted by a difficult mineral-dressing problem and they are to be congratulated on their courage and persistence in staying with it until a satisfactory solution was evolved. A visitor to the plant might have been mildly astonished, as I was, to see one type of concentrator handling that part of the load early in the 1947 season, its experimental replacement by another a little later, and then in 1948 to see that both types had simply disappeared and their place taken by the spirals which were operating as placidly as though they had been there all the time. In working out economic methods of beneficiating Alabama red ore, most of which development is still ahead of us, it is likely that we also will pass through a period of successive disappointments, for we too have a problem where it is next to impossible either to "guess 'end right in the first place," or, because full-scale operating cost is such an important factor, to lay the ultimate answer on the line in advance by means of laboratory experimentation. Iron ore being what it is instead of what it used to be, it is encouraging to have the example the authors have given us today that a tough nut that will not crack on the first blow or the second is apt to do so on the third or fourth.

Jan 1, 1950

By Ramon V. V de Araújo, Roberto B. E Trindade, Pablo R. Fica-Piras

"Lead has been reported to affect blood vessels and kidneys. It also produces adverse effects in the mental and physical development of children and nervous system of adults. It is also considered as a possible cause of cancer. Because of all these threats to the human life, the reduction of its environmental occurrence, by means of recycling, is an important additional advantage to the usual ones derived of the procedures of the secondary metallurgy: lead can be recycled several times maintaining its characteristics equivalent to the primary one.Furthermore, this way of producing the metal avoids the environmental impacts of primary lead melting. Also, as an additional advantage, it triggers the metallurgical process with a raw material in what we observe higher lead content than in the natural ores. Some of the potential sources for these purposes are: ashes, slags, electrode residues, anodic muds, spent electrolytes, solid and liquid wastes, industrial or automotive catalysts, worn-out or obsolete equipment components and/or final consumption products.About 40% of world’s lead production comes from automotive batteries, mainly composed of four parts: plastic box, electrolyte (diluted sulphuric acid), contacts and connectors of Pd-Sb and plates (PbSO4, PbO2 and PbO). The plates represent 75% of the total mass. Metallic parts can be melted at moderate temperatures and then refined. The remaining fraction, constituted by the non-metallic portions, can be recovered by hydro and electro-metallurgical routes. These routes are preferred instead of pyrometallurgical ones due to the ultimate emissions of lead particulates and sulphur dioxide.The principal constituent of the residual paste of batteries is the lead sulphate. In this process, the paste is treated in two stages: in the first, lixiviating with Na2CO3 (desulphurization of the paste), obtaining PbCO3 and Na2SO4; in the second, the lead carbonate is lixiviated with HNO3, producing Pb(NO3)2, soluble, that can be converted to metallic lead by electrolysis. The reaction of PbSO4 with Na2CO3 in aqueous solutions is fast: the global rate is limited by the diffusion of the carbonate ions inside the reaction medium."

Jan 1, 2003

By D. A. Thomas, M. F. Comerford

Poly crystalline wires of Fe-3.2 wt pct Si were cold-drawn to 31, 66, and 87 pct reductions of area. Mechanical properties and tnicrostructures were studied after recovery and re crystallization. An initial increase in strength during recovery was ascribed to strain aging, and subsequent softening was largely due to polygonization rather than re-crystallization. No unique actioation energies could be determined for the recovery process. Rather, activation energies ranged from 60,600 cal per mole at 10 pct recovery to 83,200 cal per mole when recovery was 50 pct complete. Sites for the nucleation of recrystallization were found to depend on time and temperature. In the early stages of re-crystallization, nucleation occurred in deformation hands. Later, or at high temperatures, recrystal-lized grains were nucleated primarily al grain boundaries. Polygonized structures did not seem to be preferred sites for nucleation. MUCH of the research on deformation, recovery, and recrystallization processes in bcc materials has been performed on single crystals or lightly worked polycrystals. Little study has been devoted to the relation of mechanical properties to micro-structure in polycrystals after severe deformation and subsequent annealing. This paper presents the results of a study of the tensile properties and microstructures of Fe-Si wires drawn varying amounts and annealed at a series of temperatures. EXPERIMENTAL PROCEDURE The experiments were carried out on an alloy of the following composition: 3.2 wt pct Si, 0.08 Mn, 0.016 C, 0.005 0, 0.0002 N, 0.0001 H, 0.008 P, 0.034 S. The material was received as l-in.-sq bars cut longitudinally from a hot-rolled slab provided by the Armco Steel Corp. The bars were forged to 3/8-in. rounds, centerless-ground to 0.250 in., and swaged to '0.108 in. All subsequent reductions were performed by room-temperature wire drawing at the rate of 2 in. per min. Each preliminary draft gave approximately 30 pct reduction of area and was followed by a l-hr anneal at 1010°C in dry hydrogen. Three lots of wire were made with ultimate cold reductions of 31, 66, and 87 pct reduc-

Jan 1, 1965

By T Laurencont, C Unger

The Mount Morgan minesite, located approximately 40 km SW of Rockhampton in Central Queensland, comprises 270 ha of unrehabilitated land which is the currently the major source of acid mine drainage run-off and seepage to the adjacent Dee River. Additionally, the minesite hosts an Open Cut Pit which contains 9000 ML of acidic and metal-rich water. In the absence of active management of water in the pit, there is a 50 per cent probability of an uncontrolled spill occurring in future years. The development of a contingency plan for management of overflow from the pit in the short term, has incorporated findings from numerous studies relevant to the Open Cut Pit including, but not limited to, water balance, contaminant source identification, toxicity testing, water quality profiling and limnological modelling, and estimates of probability of overflow. Extensive stakeholder consultation and peer review were also undertaken during the formulation of the contingency plan. The medium-term goal of lowering the water level in the pit to reduce the current high probability (50 per cent) of uncontrolled overflow to acceptable levels of risk is proposed to be achieved by a campaign of chemical water treatment. The treated water will be discharged to the Dee River, and sludge returned to the pit. The methodologies used for the selection and development of the water treatment process, that is proposed to involve treatment with lime, are described. Water treatment is the short- to medium-term component of a long range rehabilitation plan for achieving a negative pit water balance, and sustainable management of acidic water across the whole site. Achieving this ultimate goal will involve: reducing the inputs of water to the Open Cut Pit such that the annual water balance is zero or net negative, thus removing the need for water treatment in perpetuity; maximising, by surface rehabilitation works, the quality of run-off reporting to the Dee River; and minimising the volume of acidic seepage reporting to the seepage interception system. Possible strategies for achieving this long range goal consistent with overall site rehabilitation objectives are currently being developed and costed.

Jan 1, 2003

By William P. Lohden

INTRODUCTION It is recognized that, for a variety of reasons, some companies in the mineral industry today are by no means cash-rich and, in fact, are reporting a growing proportion of long-term debt in their capital structures. A review of recent balance sheets of small, medium-size, and some larger companies, indicates that a fair number still have substantial positions in cash equivalents such as U.S. government issues and other short-term money market instruments. In part, this paper concerns itself with companies which have sufficient cash and equivalents and/or cash generation to internally finance mining projects or expansions but which, for some reason, choose to borrow funds. Misconceptions which appear to frequently underlie so-called "leveraging" decisions are explored in this paper. Also considered arc' those circumstances under which any company, including one that is cash rich, should consider borrowing for a project in an amount beyond what would otherwise be necessary based upon its internal financing ability. I do not attempt to cover the raising of equity capital in public markets in this paper. OVERALL RETURN ON INVESTABLE CASH If you approach an individual with an investment which can be financed from savings, or by borrowing at a rate higher than one is earning on savings, that individual will quickly tell you that to pay interest at a rate higher than is being earned on savings would reduce overall income. Assuming that additional investment opportunities are not currently being considered, the individual concludes that a draw-down on savings, leaving a cushion for contingencies suited to individual circumstances, is the correct financial decision. For reasons discussed later, the simple mathematical logic leading to this conclusion tends to become obscured at the corporate level. When Leveraged Studies Are Inappropriate or Premature Surprisingly, I have heard of a number of companies that could afford to finance an investment solely with internal funds, which have made DCFROR (i.e. discounted-cash-flow rate-of-return) studies not only on a 100% equity basis but also on a leveraged basis. Certainly, a leveraged study would be appropriate if additional projects were competing for more capital than was available internally. Often, however, other projects are not far enough along to warrant a leveraged study and there is some danger that a project may be undertaken because it has an estimated acceptable rate of return, on a leveraged basis, that is not ultimately earned because some of the other projects are postponed or abandoned and borrowing is less than expected. For the above reasons, until it has been determined that (1) borrowing is a reasonable certainty for a particular project and (2) the timing and amount to be borrowed has been determined within a reasonable range of accuracy, I believe it is inappropriate and misleading to calculate DCFROR for a project other than on a 100% equity basis. Even when there are several projects currently competing for funds and borrowing will be required to finance one or more of them, using the common yardstick of calculating DCFROR on a 100% equity basis is a safer method to initially evaluate and compare the attractiveness of the projects. Many companies, whether they would have to borrow or not, will reject projects that on a 100% equity basis do not meet their minimum rate of return standards. Some companies which have to borrow will undertake a project provided the project's DCFROR on a leveraged basis meets its minimum return standards. The danger of this approach is that even moderate shrinkages of estimated cash flows could plunge return below

Jan 1, 1985

By J. L. Thompson

There are two basic forms of the LPG-slug process: the gas driven and the water driven. The pressure required for miscibility between gas and LPG prohibits the use of the gas-driven LPG process in shallow reservoirs. The water-driven LPG slug process normally exhibits good sweep efficiency. However, displacement of the LPG by water is poor. An improvement in this process appears possible by injecting a slug of carbon dioxide between the LPG slug and the water drive. Laboratory experiments were conducted in homogeneous linear systems to determine the effect of pressure on the various displacement zones. In the carbon dioxide-LPG displacement zone, the effect of pressure on the displacement efficiency is negligible above the miscibility pressure. However, the displacement efficiency decreases linearly with decreasing pressure below the miscibility pressure. With water displacing carbon dioxide, it was found that the recovery of carbon dioxide after water breakthrough can be predicted from its solubility in water. A displacement test was conducted with LPG and carbon dioxide slugs large enough to avoid interference between the oil-LPG, LPG - carbon dioxide and carbon dioxide - water displacement zones. Under these conditions, essentially complete oil and LPG recovery was obtained. However, a substantial amount of carbon dioxide was left in the core at water breakthrough. INTRODUCTION It has been shown in homogeneous linear systems that essentially complete oil recovery can be obtained by displacement with a miscible fluid such as LPG. Economic considerations dictate that the valuable LPG also be recovered. Methods proposed for recovering the LPG include (1) displacement with natural gas at a pressure high enough to make the two fluids miscible1 (the disadvantage of this method is that the required pressure of about 1,500 psi is too high for shallow reservoirs) and (2) displacement of the LPG with water2 (principal disadvantage is that a large amount of LPG remains in the formation because of poor displacement efficiency). This paper treats an improvement in the water-driven LPG slug process3,4 where carbon dioxide is injected between the LPG and water. Carbon dioxide is completely or at least partially miscible with propane and soluble in water; thus, displacement efficiency is improved at both ends of the carbon dioxide slug. To minimize effects of other variables, all experiments were conducted in linear core systems. GENERAL PROCESS DESCRIPTION The displacements of propane by carbon dioxide and carbon dioxide by water are considered separately, assuming enough of each is injected to prevent mutual interference. Displacement descriptions are confined only to the part of the pore volume containing mobile fluids unless otherwise specified. The schematic representation is given in Fig. 1. Starting at the producing well, a zone containing only oil is followed by a zone containing a single-phase mixture of propane and oil. The concentration of propane increases in the direction of the injection well and ultimately grades to pure propane. Then follows a zone containing a mixture of propane and carbon dioxide in continuously varying proportions until 100 percent carbon dioxide is reached. In this zone, the concentration of carbon dioxide in the immobile water phase also varies from zero to full saturation. Whether the displacement of propane by carbon dioxide is of complete or partial miscibility depends on pressure and temperature (Fig. 2). If the horizontal line representing the prevailing pressure intercepts the boundary curves of the phase envelopes for the prevailing temperature (i.e., if the pressure is lower than the critical

By Vincente M. Jr. Lim, Brain W. Lawrence

Underground mining operating costs consist pri¬marily of direct costs such as labor, supervision, ma¬terials, and supplies, plus indirect costs. The material and supply costs vary substantially between mines but commonly range from 35 to 60% of the total direct costs. As part of the preparation of accurate operating cost estimates for a project, information must be as¬sembled to select the material and supply items and to determine the quantities of these items that will be required. Cost data then can be incorporated with the estimated material and supply requirements to determine the total material and supply costs for the project. Estimated quantities will vary considerably between mining projects depending upon factors such as the type of material being mined, the mining method, the equip¬ment selected, drilling and blasting techniques, mucking and haulage methods, ground support requirements, number of men employed, etc. Valuable information often can be obtained from suppliers and manufacturers, including data on current operating practices for similar projects, recommenda¬tions for the specific project, and preliminary cost quota¬tions. However, quotations obtained for estimates are generally higher than the prices paid at the time of purchase. Mines operating in the area, or those mining under similar conditions, also can provide essential design information, but it often is difficult to obtain cost information from the operators. Estimated costs for the most common major items of underground materials and supplies are presented in the accompanying tables. They represent current costs or cost ranges and are intended to be used only as a guide when preparing budgetary estimates for materials and supplies. Cost data were obtained mainly from suppliers and manufacturers, with up to three quotations being ob¬tained for each item whenever possible. In most cases, as noted in the table footnotes, prices were based on quantities representing normal requirements for me¬dium-size mine operations. Every attempt was made to assure accuracy. However, the cost for most items, especially those with multiple sources, can deviate sig¬nificantly for various reasons such as geographical loca¬tion, current market conditions, quantities ordered, size of the customer (which could influence the ultimate quantities purchased), and the ability of the purchasing department. It is also for these reasons that the actual amount individual mines are now paying for specific items may vary from the estimated cost in the tables. The cost for specific sizes of items that do not appear in the tables often can be factored from the data pre¬sented. Costs for many items can be converted easily to a unit that sometimes is more basic, but not as com¬monly used, such as from a length to a weight unit. Other items not listed, such as repair parts for equip¬ment, will involve contact with suppliers to determine specific recommended requirements and to obtain costs for these items as related to each individual project. Costs are expressed in terms of US dollars as of 1978 unless otherwise specified. All measurements, sizes, and weights are expressed in conventional units (i.e. feet, inches, pounds) ; applicable metric conversion fac¬tors follow each table. Costs are represented for drill steel and bits; mining explosives; blasting caps; blasting supplies; ground sup¬port items; ventilation equipment; utility pipe, utility hose, and accessories; mine track and accessories; tires for underground equipment; lubricants and fuels; and miscellaneous supplies.

Jan 1, 1982

By Robert L. Bates

Definition An industrial mineral, says the Glossary of Geology, is "any rock, mineral, or other naturally occurring substance of economic value, exclusive of metallic ores, mineral fuels, and gemstones; one of the nonmetallics." Probably most geologists and engineers would accept this simple and straightforward definition, at least as a general statement. On analysis, however, certain anomalies crop up. For example, it may be considered arbitrary to include industrial diamond and corundum and to exclude their precious varieties, gem diamond and sapphire. So the present volume has a section on gems and gem materials, in spite of the definition. Another problem arises when we try to define precisely what is metallic and what is nonmetallic. Bauxite and ilmenite certainly qualify as metallic ores, but both are also raw materials of important nonmetallic substances; hence they are included in the book, A third anomaly is that, by common consent of geologists, engineers, mineral economists, and others concerned, the term industrial minerals may include not only rocks and minerals but also certain manufactured products like cement and lime, and even mixed groups of natural and artificial products, such as abrasives and refractories. Thus the central realm of the industrial minerals is clear enough, but its boundaries tend to be indefinable. Since a definition that allowed for every irregularity in the outer fringes would be excessively unwieldy, the one quoted above may be considered satisfactory. The expression industrial minerals is commonly equated with nonmetallics, and with the somewhat more precise phrase industrial minerals and rocks as in the title of this book. Characteristics of the Field The industrial minerals as broadly interpreted are a highly diverse group of materials; indeed, we may say paradoxically that diversity is about all they have in common. At one end of the spectrum are ordinary earth materials such as gravel and crushed stone, with a value of perhaps $3 per st; at the opposite end are industrial diamonds, which sell (by the carat) at the rate of roughly $18,000,000 per st. Neither the metals nor the fuels, and few if any categories of manufactured products, include items that differ in value by more than six orders of magnitude. Most gravel and stone are of no value unless close to a market; diamonds and other exotic substances possess such unique and desirable properties that their occurrence in remote corners of the earth is no deterrent to their use. The broad range of industrial minerals falls between these extremes of unit value and place value. The industrial minerals penetrate the entire fabric of modern industrialized society, from such fundamental operations as drilling for oil and smelting iron ore to the manufacture of virtually the whole array of consumer products. There is no industrial-minerals industry; there are many industries. The simple term field is convenient as an all-inclusive expression. An industry is considered to belong in the industrial-minerals field if its operations consist of extraction and processing, but not manufacturing. Thus the mining and beneficiation of feldspar is a mineral industry, but the manufacture of ceramic products is not. In the cement and lime industries, processing merges into manufacture, and the line is less distinct. It disappears altogether in a plant that extracts salt as artificial brines, and makes sodium and chlorine chemicals, all under the same roof. An aspect of some industrial minerals that differentiates them from the metals is that their physical properties carry over into ultimate use of the product. Such minerals as mica, asbes-

Jan 1, 1983

By Charles C. Templeton

Any explanation of the nature of multiphase fluid flow through porous media must ultimately involve a knowledge of the mechanism of such flow through the individual pores of the medium. To provide quantitative information of the latter type, a study was made of gas-liquid and liquid-liquid displacements in single uniform Pyrex capillaries with diameters as small as 4 microns. Quantitative observation of air-liquid displacements with zero contact. angle indicates the adequacy of a model based on Poiseuille's Law and the independence of capillary pressure and interfacial velocity. Consequently, this work discounts previous claims that flow is abnormally retarded in very small capillaries. For the displacement of a very viscous oil by water in a capillary initially filled with water, flow is faster than predicted by the above model. This behavior is probably due to the existence of a thin annular film of water between the oil column and the capi1lary wall as postulated by Yuster. INTRODUCTION The need for experimental observation of the microscopic nature of multiphase fluid flow, to further the understanding of the results of macroscopic flow investigations, has been previously recognized. Chatenever and Calhoun1 in connection with the API Project 47B have extensively studied the flow of fluids through layers of glass or lucite spheres between glass or lucite plates. Lowman2 prepared an interesting film concerning flow in a single capillary, using an apparatus which made a moving interface appear stationary in the field of a microscope. The purpose of the present investigation was to deter- mine what contribution might be made to this field by comprehensive quantitative observation of gas-liquid and liquid-liquid displacements in single capillaries of uniform, very small diameter. The techniques used are similar to those of Lowman but incorporate improvements necessary for quantitative work. Quantitative observations must begin with fluids of simple chemical composition to provide a basis for analyzing the more complex behavior that may be expected with natural reservoir fluids. However, some qualitative observations on systems involving crude oils are presented. Experiments of this sort involve the observation of the velocity of the interface separating two fluids, and have been performed in horizontal or vertical capillaries by several investigators.3,4,5,6,7,8 The most general treatment of their mechanics, by Brittin,9 involves forces due to capillarity, viscous resistance, gravity, an "end-drag" effect, and the rate of change of momentum of the capillary contents. Since the range of pore diameters of interest in petroleum reservoirs is about 0.1 to 100 microns, it was desired to perform these experiments in the smallest capillaries possible, to ascertain whether capillary diameter had any effect on the existing theory based on data from larger capillaries.* It was also important to be able more systematically to vary the direction and rate of displacement than was done by previous investigators. Finally, to concentrate attention on viscous and capillary forces by eliminating gravity as a parameter, this study involves only horizontal capillaries. The work of Eley and Pepper' with a "large" (0.766-mm diameter) horizontal capillary is the previous investigation which is most similar to the present method of quantitative observation. Here capillaries with diameters as small as 4 microns will be studied.

Jan 1, 1955

By K. K. Kershner, W. A. Calhoun, C. W. Funk

Future resources of aluminum may require the utilization of low grade ores to provide a more permanent protection for the nation. Aluminum minerals such as cloy, shale, and high iron laterites may become important sources. An evaluation of reserves is given. New laboratory results are reported on the Vereinigte desilication process. THIS report on future resources of aluminum metal emphasizes the necessity for investigating utilization of low grade potential ores to provide more permanent protection for the nation. Partial or complete interruption of the importation of high grade aluminum ores must be given consideration. Ultimately, aluminum minerals such as clay, shale, and high iron laterites may become the principal sources of aluminum. The development of extractive processes for treating these low grade materials is a step in long-range national preparedness that should receive more attention. In formulating such processes, the application of beneficiation methods for the purpose of classifying the several types of minerals before subjecting each type to the more expensive extractive procedures should be considered, and a careful survey of the basic factors of power sources, transportation facilities, and sources of raw material should be made. Domestic Bauxite Resources Of the domestic supply of current, treatable-grade bauxite, 95 pct comes from Arkansas. The present reserve of Arkansas bauxite suitable for metal production, including abrasive-grade, Bayer-grade, and modified Bayer-grade ores, is 34,000,000 tons. The total reserve of bauxite of all grades is approximately 75,000,000 tons. Reserves are estimated on a mined and dried basis. Data available to the Bureau of Mines in 1948 to 1949 were used in preparing Table I, which shows a breakdown by grades of bauxite for about a half of the reserves of the state. The modified Bayer ore, 10,555,500 long dry tons, is based on a cutoff of 8 to 15 pct silica. The sub- marginal 10,074,700 long dry tons is assumed to contain more than 40 pct gibbsite, more than 15 pct silica, and less than 32 pct available alumina. A considerable amount of this low grade material was consumed in 1949 and 1950. Additional tonnages of bauxitic and kaolinitic clays are indicated by the Bureau of Mines drilling project.' Applying a 50 pct factor to arrive at long tons mined and dried, the results of this project are approximately 31,500,000 tons kaolinitic clay at +35 pct Al²O3 and 11,800,000 tons kaolinitic clay at 20 to 35 pct A1,0,. Total reserves of kaolinitic clays are probably quite extensive—several times the reserves shown in the Bureau's work. Total reserves of bauxitic and high iron clays from the drilling program and previously established figures are 63,980,000 tons. The mineral dressing methods,' the lime-sinter process, he lime-sinter modification of the Pederson process," the lime-soda sinter process,"-' and the Alcoa combination processa. have been described in the literature and will not be elaborated upon here. The less familiar Vereinigte Aluminium-Werke process used by the Germans during World War 11 may require some amplification. It was used to bene-ficiate boehmite ores containing 12 to 18 pct silica for a feed to the European Bayer process. Ore was

Jan 1, 1952

By A. P. Young, F. C. Holden

IN many of the early investigations of the aging of titanium alloys, it was observed that the retained beta phase could be aged to a high hardness without an apparent change in microstructure; moreover, in some alloys it was found that even a very rapid quench produced beta having an anomalously high hardness. What appeared to be hard beta phase was designated as "beta prime," to distinguish it from the softer normal retained beta phase. Frost and co-workers'.' demonstrated that the increased hardness is caused by the formation of a metastable phase, omega, which can be identified from its X-ray diffraction pattern. This reaction also has been studied by Brotzen, et a1.,3 and the structure of the omega phase has been published by Silcock, et al.," and by Austin and Doig.3 The X-ray diffraction analysis by Austin and Doig indicated that omega is low in alloy content, approaching the composition of the stable alpha. The aging process proceeds by the path Thus, overaging results in the formation of alpha and the ultimate disappearance of omega. This is accompanied by a decrease in hardness and a recovery of ductility. The present work represents a study of the aging process in a high-purity Ti-6.4 Mn alloy, in which optical and electron microscopy, X-ray diffraction, and hardness data were correlated. The specimens, 1/8-in. sections cut from 1/4-in.-diam rod, were heated in argon to a temperature just into the beta field (810°C), held for 1 hr, and water-quenched. The aging samples were heated in air for 1 hr at 300 to 500°C. The specimens were ground and mechanically polished, finishing with alternate etching and polishing on a slow-speed wheel to remove disturbed metal from the surface. The surface finally was swab-etched, rinsed with tap water, and air-dried. The etchant used was an aqueous solution containing 1 1/2 pct HF and 3 1/2 pct HNO3. This procedure is identical with that used for preparing metallographic specimens, except that the optimum degree of final etching required for electron microscopy may vary from that used for light microscopy. Metal replicas, backed with silica, were prepared from plastic strip-pings for examination with the electron microscope. Complete details of the procedures used for preparing these replicas are available elsewhere." Fig. 1 shows a comparison between the structures revealed by the electron microscope and those obtained by conventional light microscopy. Hardness and X-ray diffraction data are listed in Table I. No evidence of a second phase is apparent in the optical micrographs for the as-quenched sample, or for the specimens aged at 300 or 400°C; fine alpha particles can be seen in the specimen aged at 500°C. In the electron micrographs, visible equiaxed pocks appear in the as-quenched specimen, and, with increasing density, in the samples aged at 300 and 400°C. After aging at 500°C, the structure becomes markedly coarser and develops an oriented appearance of a second phase, coincident with the appearance of visible alpha particles in the light micrographs. These observations are confirmed by X-ray diffraction and hardness data. In these specimens, aged for 1 hr, the intensity of the omega pattern increases to a maximum at the 400°C aging temperature, corresponding to maximum hardness and the maximum density of pocks in the electron micrographs. At this point the beta phase shows a definite enrichment in Mn. At 500°C, little or no omega re-

Jan 1, 1959

By A. D. Rich

The term "bleaching clay" or "bleaching earth," as used in the oil industries, refers to clays that in their natural state, or after chemical or physical activation, have the capacity for adsorbing coloring matter from oil. There are three common types of bleaching clays: fuller's earth, activated clays, and activated bauxite. Fuller's earth, or naturally active clay, is prepared from bentonites (see Chap. 5) that possess natural activity. It is not activated commercially; in fact, earths of this type ordinarily do not respond satisfactorily to acid activation. Fuller's earth is prepared in pulverized as well as granular form for use in the contacting and percolation processes, respectively. Acid-activated clays also are of bentonitic origin. The basic raw clay, however, is of a type that has a very low natural activity but is highly activable by treatment with mineral acid. Commercial acid-activated clays generally possess several times the decolorizing power (bleaching efficiency) of the best quality of fuller's earth. The former are prepared commercially only in the pulverized grade because of the difficulties in obtaining a satisfactory granular product, and hence are used only in the contact process. Activated bauxite is made by heat-treating bauxite ore, which in its natural state has very little natural activity. The commercial product is prepared in granular form for use in the percolation process on petroleum oils. For the most part, bleaching clay is used commercially in the decolorization of animal, vegetable and petroleum oils, fats and waxes. It is applied in two ways: (1) by the percolation method and (2) by the contacting method. Percolation refers to the passage of oil through a bed of granular clay whereas contacting refers to direct agitation of oil and pulverized clay followed by removal of the clay from the oil by filtration. In either case, the decolorizing effect is obtained by intimate contact between the liquid oil and the solid adsorbent. Petroleum oils are treated commercially by either the percolation or the contact process. Animal and vegetable oils are treated by the contact process only. Composition The raw clays from which both fuller's earth and acid-activated clays are prepared are composed of hydrous aluminum silicates containing varying quantities of magnesium, iron, calcium and other elements. These raw materials are usually nonswelling bentonites derived from volcanic ash or lava by weathering and hydrothermal chemical reactions. The bentonites have as their chief mineral constituent montmorillonite, which has the formula [(OH)4Si6A14O20•nH2O], according to Grim. (See Chap. 5, ref. 6, p. 91.) The underlying reasons are not fully known for the natural activity of the fuller's earth type of clay and its usual failure to further activate with mineral acid in contrast to the natural inactivity of the activatable type of clay. However, it may be said that the bentonites that are responsive to the acid-activation treatment generally have not undergone any drastic metamorphism. The chemical composition is not a reliable means of discrimination between a nonactive, a naturally active, and a nonactive but activable clay, therefore it is not possible to forecast the ultimate quality of a clay on the basis of the raw-clay analysis alone. Table 1 gives typical analyses of representative clays of the foregoing classifications.

Jan 1, 1960

By C. H. Gorski

A method for preparing titanium tetrachloride is described which consists of reducing rutile with coke and chlorinating the reduced product at 200° to 500°C. The crude distillate is purified by treatment with copper powder and distillation. Recoveries, exceeding 90 pct of the titanium in the rutile, were obtained. IN recent years considerable interest in metallic titanium has been aroused because of its outstanding physical and chemical properties. The present commercial processes for preparing titanium are modifications of the Kroll1 process and consist essentially of the reduction of titanium tetrachloride with magnesium in an inert atmosphere to produce metallic titanium with magnesium chloride as a byproduct. At present,' commercial titanium tetrachloride costs $0.32 a pound, which makes the price of the included titanium $1.28 a pound. As the titanium tetrachloride must be purified further before processing into metal, its ultimate cost obviously will be higher. Consequently, one of the prime requisites for the production of lower cost titanium metal is a source of low-cost titanium tetrachloride. Recently, Knickerbocker, Gorski, Kenworthy, and Starliper3 escribed a method for preparing titanium tetrachloride from low-grade Arkansas rutile by smelting the rutile with pyrite and coke to form a titanium matte and then chlorinating the titanium matte to prepare a crude titanium tetrachloride. This process had several inherent advantages. Low-grade rutile concentrates were utilized, the chlorination temperature was relatively low (approximately 200°C), and the reaction was strongly exothermic. However, this process had several disadvantages, chief of them being the rather low recoveries of titanium tetrachloride (65 to 81 pct) and the difficulty in purifying the crude titanium tetrachloride obtained. Because of the high-titanium and low-iron con- tents of rutile as compared to ilmenite, rutile should be of greater potential value as a source of titanium tetrachloride than ilmenite. Rutile, however, is not chlorinated directly in commercial practice, because reaction temperatures above 700 °C are required, at which point chlorine attacks most of the common materials of construction. The process now in use consists of converting the titanium in rutile to the cyanonitride by high-temperature reduction in an electric furnace, and then chlorinating this compound. The disadvantages of this process are the difficulty of producing the cyanonitride, the use of high-grade rutile concentrates in the charge, and the presence of several percent of silicon tetrachloride in the finished product. It would be of considerable interest to develop a new process for the preparation of titanium tetrachloride from rutile by chlorination at 200" to 500°C. Process Development Several investigators'-' have studied the reduction of titanium dioxide with carbon in an effort to prepare titanium monoxide. Invariably, the titanium monoxide formed in this manner was not pure, as it contained titanium carbide and one or more of the lower oxides of titanium. As these lower oxides of titanium are more reactive chemically than rutile, and as it is known that titanium carbide may be chlorinated readily, a study was made of the chlorination of carbon-reduced rutile. A sample of rutile concentrates from Hot Spring County, Ark., containing 76.19 pct TiO,, 5.65 pct Fe2O3, 4.18 pct SiO2, and 2.88 pct Al2O3, was used for this investigation. The experimental procedure consisted of making an intimate mixture of —100-mesh rutile and petroleum coke, adding water and molasses as a binder to foi-m a paste, charging into a graphite crucible that was covered, except for a vent to allow the

Jan 1, 1952