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Early in 1950 a new laboratory was set up to deal with problems in mineragraphy, petrology and metallography. This paper describes the equipment, the organisation and association of the laboratory with the various departments of the company, the work that has been done and future plans.At Mount Isa it was soon realised that the microscope would play a most important role in mineral dressing problems and aiding geological research.As early as 1928, R. J. Colony submitted a petrographic report on Black Star ore for Consolidated Limited; much later, in 1934-5 Dr. Grondijs published for Mount Isa Mines Limited a preliminary study of the Mount Isa orebody, followed by a mineragraphicinvestigation of mill products, and in 1937 a Study of Mount Isa Ores by H. GrondIjs and C. Schouten appeared in Economic Geology, for June-July. Other papers dealing with the petrology and mineragraphy of Mount Isa ores are appended at the end of the paper.The mill research metallurgical staff has endeavoured to incorporate mineragraphy in solving milling problems and determining the effectiveness of laboratory as well as examining minerals sent in by the geological department.For many years the amount of equipment available was limited and much of it was locally made or improvised. An improvised briquetting machine, and grinding and polishing lap gave moderate results in conjunction with an old, but serviceable, Leitz microscope. However, for more detailed and accurate work not possible with improvised equipment, many mineragraphic problems were sent to specialist in.

Jan 1, 1953

By R. B. Burt, James A. Barr, I. S. Tillotson

DISCUSSION Howard Howie (Knoxville, Term.)—The authors are to be congratulated on the presentation of a paper containing so much valuable information on the pipeline transportation of phosphate, as there is very little literature on the subject. The writer is especially interested in the paper, as he conceived the arrangement of the Akin and Godwin plants and was in charge of the design work and the engineering incident to their construction. The Akin and other phosphate deposits in the Tennessee phosphate area lie on beds of limestone that are very irregular. The limestone beds, after the phosphate matrix has been removed, are similar in appearance to land severely eroded by the action of water and denuded of top soil. Depressions in the limestone, called cutters, are irregular in depth with vertical or overhanging walls, having the general appearance of cracks in dried clay. They change abruptly in direction, width, and depth, and vary on the Akin tract from 1 to 25 ft in depth and from 1 to 50 ft in width. Pinnacles of limestone commonly occur in the cutters which appear, when exposed, like small clifflike islands in a river. Limestone floats also occur. The phosphate matrix fills the cutters and covers the uncuttered areas, the thickness of the cover varying continually and sometimes rather abruptly. It occurs generally as stratifications of phosphate rock and clay of varying thickness. The phosphate rock in the matrix varies in hardness and in percents of silica, lime, iron oxides, and fluorine, and the clay varies in toughness. In some places the deposit consists of narrow strata of rock almost devoid of clay streaks. In other nearby locations the clay will predominate. When it is excavated, the phosphate rock breaks into thin irregular lumps, locally known as plate rock. Limestone lumps are also excavated with the matrix. Akin plate rock is generally much softer than that occurring in other deposits in the area. Because of the above described physical and chemical variations of the excavated material, the resultant slurry varies in size distribution, specific gravity, and percent of slimes. When the rock is soft or when there is an increase of clay, the slime fraction is greatly increased as it passes through pumps and pipelines, resulting in reduced pipe friction. It is obvious that the longer the pipeline the greater the reduction of coarse fractions into fines, causing a decrease in pipe friction that cannot be accurately evaluated. The matrix is mined with a dragline that drops it into a hopper with a grid composed of 9-in. parallel bar spacings located above the hammer mill. The matrix on, and passing through the grid, is subject to the action of powerful sprays which wash it down to the hammer mill, together with any limestone lumps that are not removed before passing through the grid. The hammer mill reduces the feed to lumps of plate rock and clay, most of which will pass through the 8-in. pump suction. The mixture discharges into a pool containing the pump suction pipe. Water from a hydraulic nozzle moves the mixture to the pump suction intake. The pump, driven by a variable speed motor, is the same size as the pumps mentioned on p. 279. Provision is made to remove any lumps that lodge in a bend in the suction pipe in a manner similar to that used in the Florida phosphate fields. The hammer mill and pump units are mounted on wide steel skids so that they can be moved as the mining operation progresses. The discharge from the pump flows through an abrasion-resistant spiral welded steel pipe 8 1/4 in. actual inside diam, 8 in. nominal diam, for a maximum distance of 2200 ft, which is the limiting pumping distance for one pump. This pipeline, referred to hereafter as pipeline A, discharges into a ball mill without balls, which in turn discharges into a rotary screen attached to it that separates the slurried matrix into 11/4-in. oversize and undersize fractions. The oversize is returned to the mill for further reduction; the undersize is pumped to a Dorrco washer and then flows into a hydroseparator 160 ft in diam. In spite of the size reduction in the hammer mill and the blunging and washing of the slurry in its passage through the pump, pipeline, mill, and washer, the discharge to the hydroseparator frequently contains mud balls almost perfectly spherical. Sometimes the discharge from the 16,000-ft pipeline at Godwin contains mud balls the size of bird shot and smaller. This pipeline will be referred to subsequently as line B. Liquid caustic is added to the slurry at the Akin plant before its passage through the hydro-separator, which decreases the size of particles in the overflow by dispersion. In passing through pumps 1, 2, and 3 and pipeline B, the slime fraction in the underflow is increased by abrasion and blunging and also by continuing dispersive action of the caustic. The matrix for use in the experimental tests referred to on p. 279 was obtained from three small surface openings on the Akin tract that were made previous to the purchase of the tract by the Authority. Matrix used in the 2 and 4-in. experimental pipeline tests was taken from the three openings and proportioned to obtain a sufficient quantity that would be fairly representative of the average in the Akin deposits. Prospecting samples of matrix had been obtained from drill holes which showed no small variation in physical and chemical properties. Some of the physical variation is evident from the size distribution of solids in samples taken during the tests covering line B flows so thoroughly made by the Authority under the direction of Mr. Burt, see Table V, p. 280. Hydraulic gradients for a pipe of 8-in. diam were derived from the 2 and 4-in. pipeline tests using the so-called representative matrix as above described, and plotted on the profile of pipeline B. Gradients of other materials in slurry form passing through pipelines that bore some similiarity to the Akin matrix slurry were also plotted. After a study had been made of the hydraulic gradients plotted on the profile and the varying slurry flow that would probably occur during actual operation, three pumps were ordered, referred to as No. 1, 2, and 3 on p. 279. No. 1 and 2 pumps were installed and the third kept in reserve should the operation of 1 and 2 pumps prove satisfactory, since installation of the third pump would require an attendant, as well as the laying of 5400 ft of pipe to supply it with seal-water from the Akin plant. Subsequently, it was found desirable to install the third pump to maintain capacity when the slime fraction was low and the coarse fractions were large. Reference to Fig. 6 will show that the flow in B line goes upgrade in three locations. At the outlet at Godwin, the slurry flows between two 45" bends for an approximate distance of 18 ft to rise above the ground a sufficient height to discharge into a launder feeding the first classifier. This condition requires extra energy, which is taken care of by keeping the hydraulic gradient a sufficient distance above the high points. Although there are rather heavy upgrades in the line, the choking condition that might occur at the

Jan 1, 1953

By William E. Milligan

SELENIUM and tellurium occupy adjacent positions in the odd division of group VI of the periodic table immediately below sulfur, with atomic numbers 34 and 52 and with atomic weights of 78.96 and 127.61 .† A recent investigation has indicated the figures in Table 1 as the order of natural abundance of their isotopes. [ ] Experimentally, as a result of bombardment, many additional isotopes have been produced and studied. They are characterized by a relative short half-life. The elements of group VI in the periodic table are of great in-

Jan 1, 1953

By R. J. Teitel

The Pb-U system has been investigated by X-ray, thermal, and microscopic analyses. Two pyrophoric intermetallic compounds were found; UPb3 and UPb. The crystallographic structure of UPb3 is reported. A phase diagram was drawn for the system showing three eutectic and one syntectic reaction. AS a result of the interest in uranium metallurgy, the Pb-U system has been investigated. Practically no quantitative data appears in the literature concerning this system. Chips were machined from bars of high-purity uranium obtained from Ames Laboratory and the lead was 99.9 pct high-purity grade from Bel-mont Smelting & Refining Co. The chips were pickled in a dilute solution of nitric acid, washed in water and then alcohol, and dried prior to use for alloy preparation. The lead was simply sheared from the pig with no chemical treatment. Lead and uranium were placed in graphite crucibles and loaded into an induction furnace. In order to insure good alloy formation, the lead was loaded above the uranium to wash the uranium chips into the melt. After the charge was held at the desired preparation temperature for 15 to 30 min, it was allowed to cool in the crucible. The entire melting operation was accomplished in an atmosphere of helium (double charcoal refined grade with no further treatment). The procedure was to outgas the furnace by first evacuating it to 10-% m Hg, admitting helium to 8 psi gage and sealing the furnace off. An optical pyrometer focused on the charge through a hole in the crucible cover was employed for thermal measurements. Usually a 50° to 70°C correction had to be added to the instrument value. The most suitable alloy preparation temperature range was found between 1220° and 1280°C. The reason for this is explained by the phase diagram, Fig. 7. Above this temperature range two liquids separate preventing alloy formation upon cooling at a reasonable rate. On the other hand, below this range the uranium was coated with a layer of both compounds and the rate of reaction was diminished by diffusion processes. The fastest reaction rate occurred in this narrow range of temperature because only UPb coats the uranium and it evidently does not protect the uranium as well as UPb,. Apparatus and Procedures The development of apparatus and techniques was determined by the peculiar properties of the alloys. All the alloys were pyrophoric, and, consequently, the alloys had to be protected from oxidation by handling them in a dry box or inert atmosphere furnaces. Other operations performed outside of this equipment had to be done as quickly as possible. Thermal analyses were conducted in a furnace and arrangement similar to that described by the author.' Graphite crucibles having a thermocouple well in the bottom were used to contain the prepared alloy, while a helium atmosphere protected the melt from oxidation. The furnace was outgassed by pumping a 10-3 mm Hg vacuum until the furnace had been heated to 400°C. Then helium was admitted and the furnace sealed under 8 psi gage pressure. Chromel-alumel thermocouples were used for thermal analysis and the accuracy of thermal measurements was judged to be k 5°C. At first, an attempt was made to use platinum-platinum-rhodium thermocouples, but evidently lead vapors attack it at high temperatures forming low melting alloys. These lead vapors had direct access to the thermocouple because the graphite crucible was porous. A differential temperature control was used to regulate thermal analyses. The thermal gradient across an alundum tube placed between the windings and the crucible was maintained constant by a controller.

Jan 1, 1953

By Reginald S., Dean

The commercial availability of electrolytic manganese has greatly changed the position of manganese as a nonferrous alloying metal. Manganese metal commercially available up to about ten years ago was reduced with either silicon or aluminum and contained substantial amounts of the oxides of these metals and other impurities. Manganese was accordingly not available as an alloy base and its addition to copper-base and nickel-base alloys was generally limited to a manganese content of a few per cent. Several special alloys like manganin contained up to 12 pct of manganese.

Jan 1, 1953

By D. K. Crampton

NEARLY everyone who has not had the benefit of study in the field of metallurgy subscribes to a persistent and enthusiastic belief in the legendary lost art of hardening copper. This of course supplies a perfect introduction to a chapter of information on copper and its alloys, since the dissipation of fallacies and superstitions affecting an art probably constitutes the best method of getting at its real substance. Metals are hardened, but also embrittled, by a plurality of impurities. In the modern technology of copper-base metal products, we are familiar with a great host of materials, passing from one extreme of dead soft copper better than 99.9 pct pure, which in the form of wire about as thick as a match will stand hundreds of full twists in a 12-in. length, to an alloy containing less than 3 pct of alloyed substance possessing the strength of pretty good steel and capable of manufacture into razor blades, should we suddenly be deprived of steel; certainly a much better material for this purpose. Every copper alloy known to primitive man lies in some inter- mediate position and the ancient bronzes that have been found all over the world wherever an early civilization existed are usually contaminated by such impurities as sulfur, oxygen, antimony, arsenic, iron, or other materials, so that they could not possibly conform to any modern intelligent specification insuring the best combination of useful properties in alloys of their type and would go

Jan 1, 1953

By C. B. Sawyer

ALTHOUGH the element beryllium was discovered as the oxide by L. N. Vauquelin in 1797, this metallic element was not produced until about 1828, and then only as an impure powder. Thereafter the greatest single contributor to our early knowledge of beryllium was Lebeau who, in about 1899, made pure beryllium crystals by electrolysis of the fluoride and then beryllium copper by the arc-furnace reduction of beryllium oxide with carbon and copper. About twenty-five years later, under the impetus of the work done by Siemens-Halske, beryllium commenced to make relatively rapid gains in industrial importance, principally when alloyed with copper. At the present half century mark, its use is firmly established in beryllium copper and in X-ray disks of pure beryllium. Its use as a moderator in nuclear processes in piles is engaging experimental attention and might become important. Other minor uses, but increasing in interest, are in nickel-base or iron-base alloys as a strengthening agent; as a protective agent against oxidation in aluminum and magnesium-base alloys; and as a ceramic in the form of the pure fused oxide. A false start was made in the wide use of beryllium oxide as a fired fluorescent powder known as beryllium-zinc silicate, a component of the inside coating of fluorescent lamps. This application, wherein general use by the public attained some importance, was abandoned a few years ago. This action was a consequence of the uneasiness which had been generated during the past decade by the sometimes fatal health hazard to the pulmonary tract now generally attributed to beryllium and some of its compounds. Numerous law-

Jan 1, 1953

By F. H. Buttner, E. R. Funk, H. Udin

A. P. Greenough (University College, swansea, Great Britain)—I have recently made some experiments on the deformation of silver wire at high temperature in an atmosphere of oxygen-free nitrogen. The observa-tions which 1 made confirm the main conclusion of this paper, that the most satisfactory mechanism so far suggested to explain the deformation which takes place

Jan 1, 1953

By E. C. Burke, W. R. Hibbard

Plastic deformation in magnesium single crystals was studied by tensile tests at room temperature utilizing an improved preparation and testing technique. Consistent critical resolved shear stress values for basal slip were obtained. The advent of pyramidal slip at room temperature was rationalized upon the basis of grip constraints. A bend-twinning hypothesis was advanced as an explanation of mechanical twinning which occurs as a complex stress-relief mechanism. INVESTIGATIONS of the plastic deformation of magnesium have been limited to the determination of the fundamental kinetics which may be summarized as follows: 1—Twinning on the {102).l 2— Slip on the (001) plane in the [loo] direction at room temperature.' 3—Slip on the {101) or {102) plane in the [loo] direction above 225°C." 4—Critical resolved shear stresses for basal slip in tension at room temperature of 83 g per sq mm with a variation from 57 to 127 g per sq mm." Bakarian' studied the compression of thin wafers of magnesium single crystals and classified the components of the deformation mechanisms as follows: 1—The Basal field: (001) at an angle of less than 20" to the compression surface. Fracture along {101} or slip on (001) followed by {101} fracture. 2—The prism field: (001) at an angle greater than 60" to the compression surface. Twinning on the {102) generally occurring during the early stages of loading, basal slip in the areas of original orientation and (001) slip within twins. 3—The central field: (001) at angles greater than 20" but less than 60" to the compression surface. Slip on the (001). 4—The critical resolved shearing stress for {101} slip above 225°C was 400 g per sq mm. Observations of mechanical twins in hexagonal close-packed metals have been summarized by numerous investigatorsb-' emphasizing a lateral or rotational atomic adjustment, in addition to the pure twinning shear, and the importance of reorienting the basal plane to a position more favorable for continued slip, rather than the resulting small dimensional changes. Criterion for the operative twinning planes has not been clearly established. Schmid and Boas hurmised that an energy condition related to the atom movements is the determining factor. MillerQ bserved that twinning stresses in zinc crystals decreased as the amount of prior deformation increased. Preparation of Specimens Magnesium single crystals % in. in diam x 8 in. long were grown from the melt under an argon atmosphere in a gradient furnace similar to that described by Jillson." Magnesium containing 0.018

Jan 1, 1953

By C. A. Herbert

This paper sets forth the hazards of accumulations of explosive mixtures of methane and air due to inadequate ventilation, the causes of which are discussed as follows: 1. Lack of well-maintained air courses. 2. Air losses due to leaky stoppings, trap doors, and overcasts. 3. Faulty mining methods. 4. Poor supervision. A modified plan of room-and-pillar panel mine development is suggested, which, it is believed, will eliminate many off the hazards of gas accumulations inherent in the present method of mine development. It is also suggested that some water-proofing agent be used on the roof of permanent air-course entries in conjunction with roof bolting to eliminate the detrimental effect of the moisture-laden atmosphere during summer and thus prevent serious roof falls.

Jan 1, 1953

By Bunting S. Crocker

EBBLE grinding at Lake Shore is not a temporary BlE wartime substitute. The tube milling plant, with a 1000 ton per day capacity, grinds a hard siliceous ore to 90 pct — 325 mesh. The plant, prior to using pebbles, was consuming 4.3 lb of 11/4-in. grinding balls per ton of ore, which amounted to 785 tons of balls per year. At September 1951 prices, $132.60 per ton, this steel cost amounted to $104,400 per year, or $0.285 per ton milled. By the Lake Shore method of substituting screened rock for this steel, all of this cost is saved. This is one of the major economies in Lake Shore mill practice. Regardless of the ultimate price of grinding balls, a change back to steel balls is not considered. The present pebble plant is more flexible than a steel ball plant and equally efficient. For example, if it is desired to change the size of grinding media, the pebble charge in any mill can be changed completely in 4 to 5 days, as against 76 days to change completely a 1-in. steel ball charge. To change pebble size it is necessary only to change two sets of screens and clean out the rock feed storage bin. This will take 8 to 10 days as against 3 to 4 months to clean out the customary supply of grinding balls kept on hand. Also it has not always been possible to purchase all desired sizes of balls at any price. In an analysis of savings effected by the use of the pebble mills, the flexibility of the Lake Shore grinding plant should be discussed, as it has a direct bearing on these savings. The plant has always used several units to handle tonnage rather than sending all the tonnage through a single unit. This principle may result in using small diameter mills, but no objection to that is seen. At no time has any advantage been found in cost per ton ground in large diameter mills. Both the capacity and the power of any mill varies as the diameter raised to the 2.6th power. Consequently large or small mills are equally efficient, and a plant, should be designed to use as many units or combination of units as is consistent with reasonable operating practice. Mills under 5 ft diam are harder to reline, etc. To define the case at Lake Shore, 2600 tons per day formerly were milled in seven 7x6-ft ball mills and twelve 5x16-ft (and two 6x16-ft) tube mills.* This gave an excellent test plant and an extremely efficient one. In this plant the ratio of ball mills to tube mills was 1:2. When the much cheaper pebble mills were substituted for the tube mills, this ratio was changed to one ball mill to four pebble mills to take the greatest possible advantage of the cheaper operating mill, i.e., the pebble mill. This flexibility without loss in efficiency has been an important item in the cost savings. It is interesting to note that the use of pebbles for fine grinding was proved first in the laboratory in a 12-in. ball mill. In fact, since 1934 all testing on — 8 mesh material has been done in this 12-in. mill. Scope of the Tests A paper on fine grinding at Lake Shore Mines was published in July 1940.' This paper covered 7 years of intensive research on fine grinding as well as sizing methods and equipment, plant scale grinding tests on 5x16-ft tube mills with and without grate discharges both with 1-in. and -in. balls, the use of laboratory mills to evaluate plant changes, and several reports on classifiers and classification. In the following July the addendum report2 was added in which the idea of series-circuit grinding was introduced, and the results of running five stages of tube mills and bowl classifiers were shown. Since 1940, the ball milling end of the plant has been altered extensively as a result of tests on the use of 3-in. rods in 7x6-ft mills and the use of the Tyler repulping screen with from 7 to 14 mesh screens. These tests are lengthy and may be covered in a separate report later. The scope of this report is confined to ore ground by rod milling and ball milling until it passed through an 8 mesh Tyler Ty-rod screen. The —8 mesh screen undersize then was pumped to a primary bowl classifier in open circuit and the sands from the bowl sent to the primary pebble mills, see Fig. 1. In the pebble mill circuit the ore is ground to 90 pct —325 mesh (24 pct + 28 microns). In studying the flowsheet, attention should be paid to the efficiency of the classification equipment used. The Tyler repulping screen is an efficient machine on the 8 to 10 mesh separation, and the bowl classifier is equally efficient at the 325 mesh separation. Efficient classification is a necessity for series-circuit stage grinding. The ore is hard siliceous porphyry, 60 pct SiO,, 80 pct insoluble. Its grindability at different meshes has been shown near the top of the list in F. C. Bond's grindability tests.' Lake Shore is not shown, but an adjacent mine with identical ore, Wright-Hargreaves, is. Reasons for the Changeover Since 1936 grinding balls have been rising steadily in price with no sign of stopping. For a mill that used 4.5 to 5.2 lb of grinding balls for every ton of ore ground this rise represented an alarming increase in grinding costs. In many cases the quality of the grinding balls fell off as the scrap steel became more difficult to obtain. The ratio of tube mills to ball mills increased with the use of the Tyler repulping screen in the ball mill circuit. Originally only 3.0 lb of balls per ton were used in the tube mills, and this

Jan 1, 1953

By E. S. Machlin, Morris Cohen

The isothermal formation of martensite in a 71 pct Fe, 29 pct Ni alloy is found to take place mainly by the nucleation of new plates rather than by the growth of existing ones, and is dependent on the temperature and time of the isothermal hold, the amount of atherrnal martensite present, the state of internal strain, and the application of tensile stress. The conclusion is reached that the isothermal nucleation is activated by thermal fluctuations superimposed on localized regions of very high strain. The reaction-path concept, involving martensite nucleation at strain embryos by athermal activation on cooling, or by thermal fluctuations on holding, reconciles the athermal and isothermal modes of transformation, and offers a unified picture of the kinetics of martensite formation. THE phenomenon of isothermal martensite formation has been the subject of considerable study lately,'-' and its reality has been thoroughly established. The existence of such isothermal transformation has been claimed to confirm the nucleation and growth hypothesis as applied to the martensitic reaction.1 " However, the isothermal formation of a martensitic phase is also compatible with the reaction-pathw escription of the transformation. The purpose of this investigation is to examine the isothermal mode of the martensitic reaction, both theoretically and experimentally, in order to test the likelihood of the above two mechanisms. Material and Methods The alloy used in this study contained about 71 pct Fe and 29 pct Ni. The complete analysis was 29.5 ± 0.2 pct Ni, 0.036 pct C, 0.02 pct N, 0.19 pct Mn, 0.09 pct Si, 0.008 pct P, and 0.006 pct S. The amount of isothermal transformation was determined by electrical resistance measurements using a Kelvin double bridge. The specimens were in the form of rods 1/16 in. diam x 4 in. long. Aus-tenitizing was performed at 1095°C for % hr either in a pre-purified nitrogen atmosphere or in an evacuated Vycor tube, followed by oil quenching to room temperature. After this treatment, the samples were completely austenitic, and the transformation studies were conducted at subatmospheric tempera- tures. Lineal analysis and X-ray determinations of retained austenite were used to calibrate the electrical resistance changes in terms of the percentage of martensite. The martensite range curve for this alloy is given in Fig. 9 of ref. 6. The M, temperature occurs at about -18°C (255°K). Reaction-Path Theory The nucleation and growth description of the martensitic transformation that occurs isothermally has already been given by Kurdjumow.','2 However, no comparable treatment exists using the reaction-path concept." Consequently this section presents the reaction-path description of the isothermal mode of the martensitic transformation. According to the latter theory, there is a reaction path (a strain) which describes the relative motion of the atoms during their transference from the austenitic to the martensitic state. The possibility exists, therefore, that the nucleation of a martensitic plate is accomplished by an embryo that comprises a state intermediate between that of austenite and martensite. This state may be attained within a finite volume by means of a homogeneous strain of the austenitic matrix. There is a free-energy barrier (F.) along the reaction path, corresponding to a critical strain in a critical volume. When activation is achieved, a spontaneous increase in strain and volume of the embryo takes place to generate the full-size martensitic plate. This mode of nucleation is to be distinguished from the more conventional mode involving embryos of the martensitic phase that merely grow in size by an interface motion. There are two ways whereby embryos in the austenitic phase can achieve the critical state of strain for isothermal nucleation: 1—through the formation of internal strains by plastic deformation or by stress; and 2—through thermal fluctuations, preferably superimposed upon existing internal strains. The activation free energy F,, must be supplied either mechanically by internal strains or thermally by energy fluctuations, or by a combination of both.

Jan 1, 1953

By J. H. Hamilton, J. R. Lewis, J. H. Dismant, W. M. Fassell

RECENTLY this laboratory undertook the task of preparing some low carbon metallic cobalt by the carbon reduction of precipitated cobalt oxides. The oxides came in two lots and had the compositions given in Table I. Industrially, cobalt rondels' are made by the carbon reduction of cobalt oxide in small reverberatory furnaces at temperatures near but not above 1050 °C. This is a slow and tedious small batch process but does give cobalt metal which is low in carbon (1 pct C). Inasmuch as these cobalt oxides were relatively low in copper and iron it was decided to reduce them with petroleum carbon in a small three-phase electric arc furnace of about 3 to 5 Ib of metal capacity. It was hoped such a procedure would save considerable time and perhaps also indicate an improved commercially feasible process. The furnace was preheated by using small pieces of carbon electrodes to maintain the arc until a temperature of 1500°C was reached. The broken pieces of electrodes were then removed and 500 g of the cobalt oxides and 60 to 100 g of petroleum coke added. At the end of the reduction reaction, a high lime flux was added to the furnace to facilitate the removal of sulphur. Due to the fineness of the cobalt oxide powder used and also to the presence of chlorides there was considerable dust lost in charging the furnace. This was overcome by preparing briquettes composed of the cobalt oxides, charcoal, and a little bentonite to serve as a binder. The results obtained are summarized in Table 11, which shows that the cobalt metal produced in the arc furnace was high in carbon varying from 2.5 to 3.5 pct. This, of course, is much too high. For certain uses, such as in the preparation of permanent magnets, the carbon content of cobalt must be low. It was necessary therefore to find an effective method of reducing the carbon content of the cobalt that had been prepared in the arc furnace. Van Arkel3 recommends the use of Co2O3 as a means of removing carbon from cobalt. Experiments by the authors indicate that carbon is removed with difficulty by this method. Other methods used, including lancing of the molten high carbon cobalt with a jet of oxygen, proved to be ineffective. The method finally used makes use of the fact that cobalt metal is decarburized by carbon dioxide at the temperature of the molten metal. Two methods were used: 1—carbon dioxide was bubbled up through the molten cobalt, and 2— molten cobalt was maintained in a carbon dioxide atmosphere. In the first method the gas was introduced below the surface of the molten metal by means of a quartz tube. A high frequency induction furnace was used to keep the cobalt molten in both of these experiments. This kept the metal somewhat agitated and no doubt was an important factor in hastening the decarburization 'process by the second method. Both methods gave satisfactory results as shown in Table 111. An interesting observation in connection with this 'work was that a small sample of carburized cobalt metal could be decarburized by heating it with an acetylene torch adjusted to give an oxidizing flame. This may have been due to the presence of carbon dioxide in the products of combustion. Samples of molten high carbon steel were decarburized by the same method and it is suggested that nickel and perhaps manganese can be decarburized in a similar manner. Additional work, including rate studies and other theoretical aspects of this problem, is in progress in this laboratory.

Jan 1, 1953

The Mungana group of mines, in the Chillagoe district, yielded 334,000 tons of ore giving 31,831 tons of lead, 7,907 tons of copper and 3,228,600 ounces of silver. The Girofla mine produced approximately 220,000 tons of ore, and with the Lady J ane mine supplied most of the ore from this centre. The deposit was discovered in 1888, but active development did not commence from the main shaft until 1898. A subsidiary of the New Chillagoe Railway and Mining Co. Ltd., the Mungana (Chillagoe) Mining Co. Ltd., worked the mine from 1902 until 1914, selling copper, copper-lead, lead ores and fluxes to the smelters at Chillagoe. The smelters stopped operations in 1914 when the richer ores of the Girofla had been worked out and production from the Lady Jane had ceased due to heavyground and fire. The Girofla shaft was 823ft. deep with a cross-cut at 810ft. At the 710ft. level contour drives had delineated the orebody, which had been stoped about 10ft. above the level. Except for flux ores which had been stoped only for favourable smelter tariffs, the orebody was practically exhausted above the 610ft. leveL Under company ownership the mine yielded 139,265 tons of an average grade of 4.QlYr copper, 16.2% lead and 12.5 oz. per ton silver.In 1921 the Queensland Government re-opened the mine and worked it until 1927. The North Lode (Fig. 2) was discovered almost immediately at the 100ft. level and was worked down to the 410ft. leveL The ore from this branch and the completion of the stope at the 710ft. level yielded about 80,000 tons of ore averaging 0.4 copper, 9.8 lead and 7.8 oz. per ton silver during this period.

Jan 1, 1953

By Dubois Eastman

BEHIND the contrasting liquid-fuel technologies of Germany and the United States lie the basic differences of scarcity and abundance. The chemists and engineers of each nation have developed processes that accommodate available raw materials. In the United States, processing is based on an abundant supply of petroleum, which is refined into a variety of fuels and lubricants. Germany has little indigenous petroleum but has a readily available supply of coal that can be converted into liquid fuels and lubricants. As a result, in Germany several basic processes have been developed for the conversion of coal into synthesis gas (carbon monoxide and hydrogen). In turn, this gas is processed into products. As a normal function of its researches into petroleum processing, the petroleum industry in the United States has made careful studies of various conversion and synthesis techniques. A number of oil companies are carrying out independent development programs with the aim of synthesizing hydro- carbon products that can be marketed at a price that will compete with the price of refined petroleum products. American oil companies hope to perfect synthesis processes that will directly benefit the consumer. A good example of progress in these terms is the synthesis plant at Brownsville, Texas, which is based on the conversion of natural gas to synthetic fuels and other valuable products. When this plant is operated at near capacity, it is expected that the products will be able to compete favorably for the consumer dollar. The complete gasification of coal is a technique well rooted in history. As a controlled process on a small scale, it goes back centuries. As a practical technique on a commercial scale, it dates back to 1839, when "producer gas" appeared in Germany for limited industrial use. By 1873, "water gas," or "city gas" as it is sometimes called, was being manufactured commercially in the United States for use in heaters and stoves. The water-gas process was the cornerstone for modern synthesis. To older methods that were concerned only with carbon and oxygen reactions, it added hydrogen by means of steam. Thus far the goal of conversion was to produce gas for heating, lighting, industrial use, and cooking. The long step forward to synthesis was made in 1927, when Germany started to make gasoline from coal by means of the revolutionary Bergius hydrogenation process. A year earIier, Franz Fischer and Hans Tropsch had announced their process, which finally reached the

Jan 1, 1953

By A. F. van Everdingen

The pressure drop in a well per unit rate of flow is conrolled by the resistance of the formation, the viscosity of the fluid. and the additional resistance concentrated around the well bore resulting from the drilling and completion technique employed and, perhaps, from the production practices used. The pressure drop caused by this additional resistance is defined in this paper as the skin effect. denoted by the symbol S. This skin effect considerably detracts from a well's capacity to produce. Methods are given to determine quantitatively (a) the value of S, (b) the final build-up pressure, and (c) the product of average permeability times the thickness of the producing formation. INTRODUCTION Equations which relate the pressure in a well producing from a homogeneous formation with pressures existing at various distances around the well are generally used within the industry. The relation ii quite simple when the fluid flowing is assumed to be incompressible. It becomes somewhat more complicated when the flowing fluid is considered compressible so that the duration of the flow can he considered. In each case the major portion of the pressure drop occurs close to the well bore. However analyses of pressure build-up curves indicate that the pressure drop in the vicinity of the well bore is greater than that computed from these equations using the known, physical characteristics of the formation and the fluids. In order to explain there excessive drops it is necessary to assume that permeability of the formation at and near the well bore is substantially reduced as a result of drilling. completion and, perhaps. production practice. This possibility has been recognized in the literature. A method to compute the pressure drop due to a reduction of the permeability of the formation near the well bore. which is designated as the skin effect. S, is given in the following paragraphs. To start, equations normally used to describe flow in the vicinity of a well are given without considering this effect. These equations then are modified to include the effect of a skin on the pressure behavior. Finally a method is given to estimate the effect of the skin on the pressure and production behavior of a well. PRESSURE EQUATIONS Incompressible Fluid Flow If p is defined as the flowing pressure in a well of radius the pressure at distance r from the well has been shown to be:" The total pressure drop between the drainage boundary, and the well bore is given by These equations are valid only if the flow towards the well occurs in a horizontal homogeneous medium and the fluids are incompressible. The assumptions imply that all fluid taken from the well enters the system at r a condition rarely encountered in practice. Compressible Fluid Flow, Steady State A more realistic equation is obtained if it is assumed that the compressibility, c, of the flowing fluids is small and has a constant value over the pressure range encountered. After the well has been producing for some time so that its rate has become constant and steady state is reached, the pressures throughout the drainage area are falling by the same amount per unit of time, and the pressure differences between a point in the drainage area and the well are constant. When these conditions are met. the rate of production, q, from a well is equal to where dp/dt is the pressure drop per unit time. The fluid flowing at a distance from the center of the well is equal to From the last equation and from Darcy's law it can be shown that The equation holds for a depletion-type reservoir of radius drained by a well located in its center, provided the compressibility of the fluid per unit pressure drop is small and constant, and no fluid moves across the boundary Compressible Fluid Flow — Nonsteady State Table 111 of reference (5) shows the relationship between the pressure at the well bore and the reduced time, The pressure-drop function, p represents the drop below the original reservoir pressure, p caused by unit rate of production for several values of R, the ratio of drainage boundary radius to well radius, r In most reservoirs the values of approach infinity. and under these conditions the values of p shown in Table I of reference (5) can be used where p then signifies the difference between the pressure in the well and the prevailing reservoir pressure per unit rate of flow. The total pressure drop below prevailing reservoir pressure amounts to where the factor converts the cumulative pressure drop per unit rate of production to cumulative pressure drop for actual rate. q. For values of T > 100 the P function may be written (equation VI-15 of reference 5) as Using the time conversion the difference in pressure between reservoir and well becomes If values for the physical constants of the formation and the fluids are inserted, it is found that T exceeds 100 after a few seconds of production (or closed-in time), so that the approximation becomes valid almost at once. A simple relation between the pressure in the well and in the reservoir can also be derived by considering the well as a point source"" '" instead of a unit circle source, that is, by using Lord Kelvin's solution instead of the unit circle source

Jan 1, 1953

By M. E. Hassan, J. C. Calhoun, R. F. Nielson

An apparatus was constructed for the measurement of inter-facial tensions over a range of temperatures and pressures. This apparatus utilized the pendent drop method, and resembles in construction similar apparatus recently described in the literature and in use in some petroleum research laboratories. The interfacial tensions of benzene, propane, n-pentane, n-hexane. n-octane. and iso-octane against water were measured at temperatures ranging from 26" to 82" C and at pressures ranging from 1 to 204 atm. Values of interfacial tensions for the henzene-water system and their variations with temperature and pressure are generally in good agreement with value? of previous investigations. The data in all cases showed a slight decrease of interfacial tension with pressure at constant temperature in the range studied. The effect of pressure became less as the pressure was increased, with an indication of a reversal of the effect at higher pressures. There was a decrease of interfacial tension with temperature at constant pressure in all cases, as would normally be expected. This rate of decrease became greater the higher the temperature. A general equation is presented for the interfacial tensions as a function of presPurp and temperature over the range studied, and the constants calculated for each system. A definite trend was found in the effect of molecular weight on the interfacial tension at a given temperature and pressure, for the homologous series from propane to n-octane. Data for n-decane from the literature fitted well into this trend. INTRODUCTION It has been recognized for many years that surface forces play an active part in the production history of an oil reservoir as well as in determining the amount of unrecoverable oil. The magnitudes of these forces are governed by the values of the interfacial tensions. These vary greatly with composition, pressure, and temperature. The effect of composition is greater than that of pressure and temperature over the ranges normally encountered. In fact, because of the variety of compounds present in a crude, no attempt has yet been made to correlate crude composition with its surface tension or with its interfacial tension against water. The amount of dissolved methane greatly affects the surface properties of an oil, and there are "surface-active" compounds in crudes which have a much greater effect on boundary tensions than do equal amounts of hydrocarbons. The purpose of the present work was partly to contribute data that would eventually be used in correlations applicable

Jan 1, 1953

By Frank C. Kelton

It is perhaps not widely realized that extraction and saturation processes carried out on oil well core samples alter the properties of these samples to varying degrees. On the other hand it is felt by some that quick-freezing of core samples increases their permeability and porosity significantly. Accordingly, laboratory tests were carried out on 49 pairs of horizontally adjacent samples in order to differentiate between the effect of quick-freezing per se on permeability and porosity of the samples, as distinguished from the effect of the identical saturation treatment on permeability and porosity of the companion samples. Also, additional field data were obtained on comparison of frozen vs unfrozen companion samples. LABORATORY INVESTIGATION OF FREEZING us SATURATION EFFECTS Procedure The samples used in these tests were two-cm cubes cut in horizontally adjacent pairs from cores from eight Gulf Coast and Mid-Continent wells, which cores had not previously been frozen. These samples were extracted with carbon tetrachloride, dried, and air permeabilities run in the conventional manner. They were then evacuated and saturated with brine of 25,000 ppm sodium chloride content, and porosities determined by gain in weight. The samples were partially desaturated by evaporation down to an average brine saturation of 68 per cent. One sample from each pair was quick-frozen by covering with dry ice after wrapping in a single layer of paper, and allowed to remain frozen for about two hours; the companion sample from each pair was not frozen. After thawing the frozen sample, all samples were immersed in tap water overnight in order to leach out most of the brine. Air permeabilities were re-run, and the samples were again saturated with brine to determine a second porosity value. For purposes of averaging of data, the samples were grouped according to four permeability ranges, from 0 to 10, 10 to 100, 100 to 1,000, and 1,000 to 3,840 md. Average permeability and porosity changes for the frozen vs the unfrozen adjacent samples are shown in Table 1. Discussion As may be seen from Table 1, the averages of the per cent permeability increases for the quick-frozen samples ranged from 3.8 to 12.9 per cent among the four permeability groups. The average changes among the four groups of unfrozen companion samples ranged from a decrease of 0.2 per cent to an increase of 9.3 per cent. There was no particular correlation of these changes with magnitude of permeability; however, the increase for each group of frozen samples paralleled the increase for the corresponding unfrozen samples. The differences between the two sets of values are believed to be a valid indication of the effect of the quick-freezing in itself, since the treatment of the two samples in each pair was identical except for freezing. The permeability changes which are strictly the result of the quick-freezing are shown in the sixth column of Table 1. These range from a decrease of 0.9 per cent to an increase of 4.0 per cent; the overall weighted average is 1.2 per cent, as compared to an average increase of 6.8 per cent caused by the saturation treatment of the samples not frozen. The average porosity changes are in general smaller than the changes in permeability, and range from a decrease of 2.3 per cent to an increase of 3.3 per cent. The overall weighted average change ascribed to the quick-freezing is 1.0 per cent of porosity. Many factors can contribute to the changes in permeability and porosity observed when subjecting cores to the simple processes used in these tests. Such are: hydration and swelling of clay, adsorption of ions, changes in surface structure and wettability, expansion and compression effects due to ice formation, shrinking and cracking, leaching of salts and colloids, displacement of particles resulting in either blocking or enlarging of pore openings. Whatever particular mechanisms are involved. however, it is apparent not only from this study but also from other investigations in the literature' not directly concerned with quick-freezing, that the effects produced by commonly used extraction, saturation and drying techniques may be of considerable magnitude The results of this study indicate that for the particular samples and techniques used, such effects are of the order of five to six times the effect of quick-freezing. insofar as changes in permeability are concerned. It may be argued that these samples might not include extremely shaly material where the effect of freezing upon permeability may be much greater. However, had such material been available for these tests, it would undoubtedly have been very susceptible also to alteration by the extraction and saturation treatment used. To investigate this point further, the individual sample data were re-grouped according to the magnitude of the average per cent permeability increases for the pairs of samples, irrespective of permeability. The results

Jan 1, 1953

By H. G. Doll

A new electrical logging method. called MicroLaterology is described. whereby the resistivity R of the invaded zone close to the wall of the bore hole is measured. This method essentially utilizes a system of concentric circular electrodes iml,edded in an insulating support which is applied to the wall of the hole. A beam of current of very small diameter is focused horizontally into the formations by means of an automatic control device. and then opens widely at short distance from the wall. with this method, R most often can be recorded directly. except when the mud cake is very thick. in which case a correction is easily provided. The basic role of factor R in the quantitative analysis of electrical logs in terms of fluid saturation and of porosity is explained. The paper is illustrated with field examples. INTRODUCTION In electrical logging. the resistivity of that part of the penneable and porous formations which is invaded by mud filtrate is an important factor in the interpretation. Measurements made with the conventional devices — normal. lateral — and also with improved systems as the Laterolog and induction logging' — are very often more or less affected by the presence of the invaded zone. and the knowledge of the resistivity of this zone is useful in the evaluation of the true resistivity of the beds. which itself is a basic element for the determination of fluid saturation. Moreover. the comparison of the resistivity of the invaded zone with the resistivity of the mud filtrate gives valuable indications on the magnitude of the formation resistivity factor — which in turn is necessary for the quantitative interpretation of the logs. both in terms of fluid saturation and of porosity. On the other hand. it is generally admitted that the invaded zone is not a homogeneous medium separated from the uncon-tamirlated part of the bed hy a well defined cylindrical boundary. but that the fluid distribution—filtrate. connate water. hydrocarbon — and hence. the resistivity. in the invaded zone varies progressively with the distance from the wall of the hole. The term "resistivity of the invaded zone" therefore corre-sponds to an average value which is a function of the distribution of the fluids Inasmuch as the law of this distribution is not exactly known, the resistivity of the invaded zone is not a well defined factor. A much better definition is obtained if the medium under consideration is limited to that part of the formation which is within a short distance from the wall of the hole. It seems likely a within a distance of at least two or three in., most of the fluids in in the pores of tile formation have been displaced by the mud filtrate. The connate water has almost certainly been flushed out. and the oil. if any has generally been reduced to a comparatively small amount. The resistivity witliir~ the radial limit of two to three in. is. therefore. prac.tically constant at an). given level: its value. at least when the proportion of conductive solids in the formation is negligible. is chiefly dependent on the resistivity of the filtrate and on the porosity of the formation, and is affected only to a relatively small degree by the presence of the small amount of residual oil. This part of the formation close to the wall of the hole will he designated in the following as the "flushed zone." a-distinguished from the more general term of "invaded zone'. which relates to the part of the formation extending from the wall out to the distance where the formation is completely uncontaminated. The symbol R,, will he used for the resistivity of the flushed zone. (The notation R is related to the radial distance from the hole. If x designates this distance. xo is the initial value of x, i.e., the value corresponding to the region very close to the wall.) The determination of R is difficult, if not impossible. from logs made with the conventional devices. The long normal and the long lateral are. of course. not suited for this purpose because their radii of investigation are by far too large. The short normal. and the limestone sonde—-after correction for the effect of the hole hole — give resistivity values which corre. spond to materials situated within a comparatively short distance from the hole, but this distance is still several time. as great as the thickness of tire flushed zone. The only value which can be obtained with these devices corresponds to an average resistivity of the invaded zone- — and this only provided the invasion is deep enough, since otherwise the meas "red values would also be affected by the uncontaminated region beyond the invaded zone. It should nevertheless be recalled that despite these limitations. the measurements given by the short normal and or the limestone sonde are always very useful for qualitative interpretation. and also in favorable cases for the qantitative analysis of the logs in terms of saturation and porosity. The MicroLog. which was primarily developed for the detection of permeable beds and for an accurate determination of their boundaries. provides a good approach towards the evaluation of R. In the case of hard formation.. however. The

Jan 1, 1953

By H. J. Mutz

THE International Nickel Co. of Canada Ltd. operates five underground mines and an open pit. Four of the mines, the Frood-Stobie, Creighton, Murray, and Garson, are on the south range of the Sudbury Basin, map above, within a radius of 10 miles of the city of Sudbury, Ontario. The fifth mine, the Levack, is on the north range of the Sudbury Basin, 30 miles to the northwest of the city. The open pit is operating on surface ores of the Frood-Stobie orebody.

Jan 1, 1953