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By E. Maxwell, C. J. Bechtoldt, H. C. Vacher

IN the course of an investigation of the properties of metals at low temperature there was occasion to determine the constitution of four iridium-osmium alloys. There is very little information in the literature1 on the constitution of synthetic Ir-0s alloys. Zvyagintzev' s has made a comprehensive study of different natural Ir-0s alloys and concludes that alloys containing more than 32 pct 0s have the close-packed hexagonal structure of osmium, whereas those containing less than 32 pct 0s have the face-centered cubic structure of iridium. The alloys studied in this work were prepared by the American Platinum Works, Newark, N. J., and were received in the form of fragments approximately 1.5 mm average diameter. The fragments had been obtained by crushing ingots made by fusing charges of iridium and osmium under an arc and air cooling. The ingots were not given a homogenizing heat treatment. Sample fragments Table I. Results of X-Roy Diffraction and Microscopic Examinations Phases Present as Determined by X-ray Diffraction Osmium Alloy Close- Iridium Face- Packed Centered Osmium, Iridium, Hexagonal Cubic Mlcro- WtPot Wt Pct Structure Structure scope 0 99.9 None Present 1 23.6 76.4 None Present 1 38.7 61.3 Present Present 2 59.4 40.6 Present Present 2 79.0 21.0 Present Not detected 2 99.9 0 Present None 1 Note: Chemical analyses of the iridium, osmium, and alloys were furnished by the American Platinum Works. of the iridium and osmium used in making the alloys also were included. Several fragments of each metal and alloy were examined microscopically and by X-ray diffraction. For the X-ray method the fragments were crushed further to pass a 270-mesh screen, then sealed in evacuated fused-silica tubes, heated to 1100°C for 18 hr, and allowed to cool in the furnace. Powder X-ray diffraction patterns were obtained from the annealed fragments by means of a Norelco camera having a diameter of 114 mm, and unfiltered cobaIt radiation. For the microscopic examination several fragments in the as-received condition were mounted in Melmac, (American Cyanamid Co.) and ground using the conventional series of abrasive papers. The polishing was done with 0-2 diamond abrasive on a Microcloth (Buehler Ltd.) lap, wet with xylene. After polishing, the surface was etched electrolytically in a 10 pct solution of chromic acid or in a 10 pct solution of potassium cyanide. Both reagents attacked the osmium-rich constituent, whereas the iridium constituent was attacked slightly by the chromic acid reagent and not noticeably by the potassium cyanide reagent. The results of the X-ray diffraction and microscopic examinations are summarized in Table I. Fig. 1 shows the microstructure of a 21 pct Ir-79 pct 0s alloy. The results indicate an appreciable solid-solu-bility range of osmium in iridium as was reported by Zvyagintzev.' The solid-solubility range of iridium in osmium is more restricted, apparently less than 21 pct Ir. This implies a large range of composition in which two phases can coexist that was not reported by Zvyagintzev.

Jan 1, 1955

By O. B. Bennett

WHEN diamond drilling was introduced in the Rhokana mines in 1939 it was used principally for pillar removal and for completion of the upper portions of shrinkage stopes which were being affected by increasing pressure. This method of drilling long blastholes proved so successful that it was extended gradually to cover stoping, pillar recovery, and hanging cave work. BY 1949 virtually all the ~roduction of Mindola and Nkana was being obtained by this method. At the present time 87,500 ft are drilled each month by the 80 diamond drills in daily operation. Responsibility for control and issue of diamond drilling equipment and crowns, as well as tabulation of all performance figures, was taken over by a sPecially formed Roto drill department, which also investigated the problems encountered with this new method. To assist this department a fully equipped test chamber, Fig. 1, was established underground where performances of various types of machines and equipment could be studied under conditions as nearly uniform as possible. Since the establishment of this department, which was eventually taken over and incorporated into the study department, considerable experimental work has been done on every aspect of the subject. The problems can be classified broadly under four headings: improvement of drilling equipment, crown design, machines, and stoping layouts. One of the major problems with drilling equipment has been to eliminate vibration. Owing to flexing of rods in the hole, severe friction is set up on the back end of the 'Ore barrel and On any high spots in the rods, inducing harmonic vibration in the string of rods and causing the crown to chatter against the face. This not only causes premature crown failure but also reduces penetration speeds and increases wear on the machines and rods used. In the early days, when only holes of EX size were drilled, vibration was largely overcome by periodic greasing of rods and core barrel during each run, but with the change-over to the larger BX hole it became obvious that application of grease by hand was inefficient and time-consuming, and attempts were made to perfect a self-lubricating core barrel. A series of these core barrels was made up and tested and a number of the latest type were used under normal operating conditions, but although footages up to 120 ft were drilled without refilling the overall performance was inconsistent, and the idea was shelved in view of the success of the stabilizer rods referred to later in this paper. At the same time tests were made with barrels 5 ft and later 6 ft long instead of the normal 2 ft. Although a slight improvement was noticed, greasing was still necessary. It was found that rod vibration increased as the core barrel became worn, and in an early test chamber experiment crowns drilled with a worn core barrel averaged 95 ft with a diamond loss of 4.76 carats, whereas the same type of crowns with a new barrel averaged 228 ft with a diamond loss of 3.13 carats. until then all BX drilling had been done with B-sized rods, but during a test on a string of BX-sized rods it was noticed that vibration was negligible. Because of the larger surface area of metal bearing on the sides of the hole, however, the friction and resistance of rods of this size rendered them impracticable on any but the most powerful of the machines, The use of stabilizers spaced evenly along the rods was the next logical step, and for this B couplings, see Fig. 2, were set with three tungsten carbide inserts 1 in. long placed around the periphery equidistantly and at an angle of 45" with a right hand lead. These were placed immediately behind the core barrel and then at 12-ft intervals, as it was found that vibration still occurred when the stabilizers were more than 15 ft apart. The effect of these stabilizers was immediately noticeable; holes were drilled with a minimum of vibration, penetration speeds were improved, and as it was no longer necessary to grease the rods there was a marked decrease in the overall drilling time for each hole. While tests were being made with the stabilizer comeb periodic were taking place with a set of tapered threaded rods, and because there was marked improvement in efficiency it was decided to incorporate the stabilizers and tapered threading in all new rods ordered for Rhokana. The feature of these rods is that only four full turns are required to tighten the coupling as against nine for the present type of B rods. Also, as they are self-centering it is virtually impossible to crossthread them. Each rod has a male 5" tapered Acme thread, Fig, 3, on one end and a female at the other, so that separate couplings are unnecessary, and every fifth rod has an

Jan 1, 1955

By F. C. Langenberg, R. W. Lindsay

COPPER sometimes is added to steel and cast iron as an alloying element to improve or impart specific properties. However, in some steels it exerts an impurity effect in impairing response to fabrication by hot working and deep drawing. The resid-

Jan 1, 1955

By William Y. Holland, Roger H. Cook

Dexter H. Reynolds (Chapman and Wood, Mining Engineers and Consulting Geologists, Albuquerque, N. M.)—A number of questions are raised by conclusions and inferences made in the above-mentioned paper. The more troublesome of these concern use of the various pozzolans to combat the deleterious effects of the alkali-aggregate reaction. The most alkali-reactive materials listed are opal and rocks containing opaline silica. The pozzolans mentioned specifically for use as amelioratives are opaline shales and cherts. These are stated to retard the expansion caused by the alkali-aggregate reaction. Another well-recognized pozzolan is diatomaceous earth, which consists principally of opaline silica. A pozzolan presumably owes its effectiveness to its high reactivity with the alkaline liquid phase of the concrete mix. It appears reasonable to expect that finely divided opaline silica added as a pozzolan would be more susceptible to reaction with the alkalies present than would larger particles of the same material. The authors report that work with high and low alkali cements indicates that in the presence of alkali-reactive materials, deleterious expansion depends upon the alkali content of the cement. The total effect, therefore, should be more or less independent of the amount of reactive aggregate present, and still more independent of its state of subdivision. The deleterious effects should, if anything, be aggravated by the addition of a finely divided, highly reactive pozzolan. Further, if the alkali-aggregate reaction is of great importance in the long-term soundness of concrete structures, the addition of a pozzolan to a concrete made with aggregate free from known deleterious materials would be a questionable procedure. The benefits reportedly accruing from such use of pozzolans are greater ultimate strength for a given cement content, increased resistance to deterioration by exposure to sulphate solutions and other mineral waters, and greater resistance to damage by wetting and drying and freezing and thawing. In view of the deleterious effects of highly reactive materials are these benefits ephemeral? The same considerations apply to another alkali-reactive material, chalcedony, which appears to consist of ultrafine-grained quartz, with opal absent in detectable amounts. Quartz flour is notably reactive chemically and physiologically (cf. Ref. 11 of Holland and Cook's paper), a fact borne out by its effectiveness as a pozzolan, which presumably might be expected to offset the deleterious effects of the presence of chalcedony in the aggregate. A second question of some importance concerns the reportedly highly deleterious reactivity of acidic and intermediate volcanic glasses, such as rhyolite, perlite, and pumice. Air entrainment is listed as one of the ameliorative measures to combat the deleterious effects of the alkali-aggregate reaction. The alkalic-silica gel formed by the reaction may expand into air bubbles and thus not cause appreciable expansion of the concrete mass. It would appear then that pumice and perlite, particularly perlites of the pumiceous types and other types after expansion, would also tend to counteract the expansion, since these materials consist largely of voids and air bubbles. Certainly this would be expected of structural concrete in which pumice or perlite is used as total aggregate. Finely ground pumice, perlite, and volcanic ash have been demonstrated to be active pozzolans (cf. Pumice as Aggregate for Lightweight Structural Concrete by Wagner, Gay, and Reynolds, Univ. of New Mexico Publications in Engineering No. 5, Albuquerque, 1950). In fact, the term pozzolan was first associated with finely divided pumice or volcanic ash. Such materials were used with hydrated lime as the sole cementitious agent in constructing public buildings, roads, and aqueducts by the ancient Romans. The deleterious alkali reactivity of the volcanic glass, itself containing several percent of the alkalies, apparently did not contribute to the remarkable state of preservation of those ancient structures, as exemplified by the Appian Way and the Pantheon Dome. Still a third question involves .the reactivity of constituents of concrete when exposed to various salt solutions. Resistance to. deleterious expansion and cracking as a result of contact with mineral waters and its relationship to the mineral content of the aggregate are not mentioned by the authors. Yet the phenomena pictured in Fig. 1, and especially in Fig. 2, appear very much like those caused by exposure to mineral waters. The deterioration of concretes exposed to sulphate waters is generally considered related to the chemical constituency of the cement itself, particularly to the relative amount of tricalcium alum-inate contained. Could not many of the ill effects presently blamed on alkali-aggregate reaction really have been caused by contact with sulphate or other salt-containing mineral waters? Or perhaps their use as mixing waters? May not the deleterious expansion be as much a function of the chemical makeup of the cement as it is of the mineral constituency of the aggregate? Would it not be just as important to use alkali-free mixing water as it is to use a low-alkali cement? It appears obvious that resistance of cements and concretes to sulphate and other salt solutions cannot be left out of account in discussion of deterioration of concrete structures with time. This factor may be of equal or even greater importance than the alkali-aggregate reaction, particularly for concrete subjected to wetting and drying cycles, such as airstrip paving, water-retaining dams, and highway structures. Another very important factor is called to attention on page 1022 of the article in Mining Engineering, October 1953, in that failure of concrete structures may result from poor construction practices and use of too high water-cement ratios. Both of these can contribute remarkably to decreased resistance to attack by sulphate waters, and presumably could have an equally remarkable effect upon extent of damage resulting from the alkali-aggregate reaction. From the above remarks it appears that while alkali-aggregate reaction may be an important factor in decreasing the useful. life of a concrete structure, it is not the only factor involved, and it may not be even a controlling factor. Likewise, many of the phenomena apparently associated with the alkali-aggregate reaction may have resulted from cond'itions which had little relationship to the alkali-reactivity of a constituent of the aggregate. Certainly if alkali-aggregate reactivity is a major factor in bringing about early failure, one cannot help feeling anxiety concerning the future of the many concrete structures in this country and abroad in which pumice and perlite were used as total or partial aggregates. This anxiety can only be dispelled by calling to mind that among the best-preserved relics coming down to us from ancient times are structures made with mortars containing highly alkali-reactive aggregates.

Jan 1, 1955

By Irving Hartmann

Several recent ignitions of firedamp - a mixture of methane and air - in American coal mines have been attributed to frictional heating when hard rocks were struck while cutting and drilling coal seams. Although none of these ignitions caused severe explosions, they call attention to a problem that can become increasingly significant as mechanized mining is developed further. The power in and rapid release of energy from high-speed machinery has increased the rates of advance into virgin coal creating many problems. Unforeseen faults and hard mineral inclusions may be encountered; coal brought down in this way is finer in size; more gas is released from the seam; it is frequently more difficult to provide adequate ventilation at the' face; and new roof-support problems must be solved. In particular, continuous mining machines (also known as continuous miners) greatly increase the frequency of contact between cutter bits and minerals. In view of these conditions, it may be expected that more gas ignitions will occur as a result of frictional heating unless the situation is understood and remedial measures are introduced. The problem of frictional heating is not new in coal mining. In Europe, particularly in England, it has been a concern for more than a century. During the last 15 to 20 years frictional ignitions have been a major cuase of explosions in British mines. Explanations for the greater number of such ignitions in England may be the special character of the coal measure strata, the mining methods, the rate of gas emission and possibly its composition, and less effective ventilation near the face. To reduce the ignition hazard, considerable laboratory and field research has been conducted, particularly by the Safety in Mines Research Establishment, Ministry of Fuel and Power of Great Britain. Much of the information presented in this report has been drawn from these studies.

Jan 1, 1955

President-Mrs Robert D Coombs, 375 Paramus Road, Paramus, N J First Vice-President-Mrs Howard R Norsworthy, 333 East 53 Street, New York 22, N Y Second Vice-President-Mrs Arthur Notman, Circle Road, Dongan Hills, Staten Island 4, New York Third Viee-President-Mrs David Eugene Park, 30 Sutton Place, New York 22, N Y Fourth Vice-President-Mrs Cony T Brown, 211 East Abeyta Avenue, Socorro, New Mexico Fifth Viee-President-Mrs J A Carpenter, 245 University Terrace, Reno, Nevada Recording Secretary-Mrs W McG Peirce, 7 Lexington Avenue, New York 10, N Y Asst Recording Secretary-Mrs Arnold H Miller, 601 West 115 Street, New York 25, New York Corresponding Secretary-Mrs Theodore Nagel, 76 Remsen Street, Brooklyn 1, New York Treasurer-Mrs Robert W Rowen, 116 East 68 Street, New York 21, N Y Assistant Treasurer-Mrs Samuel H Dolbear, 11 Broadway, New York 4, N Y Assistant Treasurer-Mrs H A Kursell, 12 Murray Hill Road, Scarsdale, New York

Jan 1, 1955

By J. N. Anderson

Developments in reverberatory furnace practice at Noranda over the period 1928 to 1953 are described. Features of interest are increasing furnace tonnage from 700 to 2000 tons per furnace day, the use of the suspended basic roof, and improvements in furnace fuel ratio. Points of comparison and contrast between Canadian and American furnace practice are given. OPERATIONS at the Noranda smelter have been described in a series of papers published between 1930 and 1945.1-4 In the present paper the development of reverberatory furnace practice over the 25 year period from the beginning of operations up to the present time will be reviewed and current furnace practice will be described in some detail. Particular attention will be given to those features which are characteristic of Canadian practice: first, the use of the suspended basic roof; second, the deliberate driving of furnaces to give tonnages in the range of 1400 to 2000 tons of solid charge per furnace day; and third, the continuous operation of furnaces at high tonnage for many years without any extended shutdown for repairs or rebuilding. Finally, points of comparison and contrast between reverberatory furnace practice in Canada and the United States will be discussed. The Noranda smelter, which started in December 1927, was built for the reduction of ore from the Horne mine where early development had shown a comparatively small tonnage of rich cop-per-gold ore of a grade and character which would require direct smelting. The smelter was designed for a capacity of 1000 tons of ore a day and originally consisted of eight roasters, two reverberatory furnaces, and two converters, together with necessary auxiliaries. The discovery of a large new body of ore in 1928 made it necessary to increase both the size and the scope of the reduction plant. A mill which was ultimately brought to a capacity of 3000 tons a day was built for concentrating low grade ore and in addition the capacity of the smelting plant had to be greatly expanded, so that for the next fifteen years every effort in the smelter was directed toward achieving maximum tonnage. Because the layout and design of the smelter made it impracticable to add a third furnace, it was necessary to increase the tonnage on the two original furnaces by improvements in furnace design and operation, roasting and converting equipment being added as required to meet the demands of increased furnace capacity. The smelter tonnage, which reached a peak in 1941, was curtailed in 1944 when it became necessary to operate on a one-furnace basis because of a reduction in the output of the Horne mine due to a shortage of labor. Two-furnace operation at a moderate tonnage was resumed in 1949. In the early years the smelter tonnage was made up almost entirely of Noranda ores and concentrates. However, since 1937 an increasing tonnage of ores and concentrates from other mines has been treated in the smelter. In recent years, with decreased production from the Horne mine, copper concentrates from several mines in the district, treated on a custom basis, have formed an important part of the smelter tonnage. A review of developments in reverberatory furnace practice at Noranda falls naturally into the following four periods: 1—1928 to 1935, the early years; 2—1935 to 1944, the period of greatest change and development; 3—1944 to 1949, one-furnace op-

Jan 1, 1955

By W. A. Boyer

Edward Thomas (U.S. Bureau of Mines, Washington, D. C.)—This excellent article on an ingenious and successful installation of wooden rock bolts loses much of its effectiveness through an attempt by the authors to establish the general adaptability of this type of support. Possibly because they have only local experience as a guide, they imply erroneously in the first paragraph that the Bureau of Mines has been opposed to wooden bolting, although later in the article reference is made to a Bureau publication on the subject. In 1947 the Bureau of Mines decided to sponsor experiments in roof bolting in coal mines because the experience of the St. Joseph Lead Co. had indicated that this type of roof support appeared to be a roof-fall accident-prevention measure that might be adopted and also effect economies in operating cost. Justification for this belief has been borne out, particularly in coal mining. This program has been carried out under the following general program: 1—The Roof Control Section of the Bureau of Mines has advocated and initiated underground experiments under controlled conditions with many different ideas related to rock bolting since 1947. In no instance has cooperation in developing an idea been refused, no matter how ridiculous it may have seemed at first glance, if it has been requested by a mining company. 2—The Bureau of Mines has no police powers over the selection of roof-support devices and seeks none. 3—At the request of an operator, the Bureau of Mines will make comparative tests on various types of bolts underground and will submit resultant data for the operator's consideration. 4—Wherever possible, the Bureau publicizes successful installations, so that others may benefit from this experience; however, it is careful not to discriminate between manufacturers of bolts or bolt-installation equipment. Unsuccessful experiments probably should also be publicized, but from a practical standpoint it is usually not feasible. In other words, the role of the Roof Control Section of the Bureau is in line with the original purpose for which the Bureau was first organized: to serve industry through gathering, analyzing, and disseminating factual data. It would seem to be logical that the starting point for any experimentation on roof bolts in coal mines should be the time-proved practice of the

Jan 1, 1955

By H. R. Brannon, F. M. Perkins, Weldon O. Winsauer

Both the abnormal resistivity exhibited by shaly reservoir materials and their potential are due to adsorption of ions. Interrelationships between the two have been derived and verified by laboratory results. These relations which have resulted from this work may be used in a qualitative manner to estimate whether or not a particular shaly reservoir contains hydrocarbons, and also to estimate the porosity of shaly sands. INTRODUCTION In spite of the progress which has been made in the last decade toward a better understanding and utilization of the electric log, there remain a number of problems in the interpretation of the log. One of these which is often troublesome is that of divining the nature of the fluids in sandstones or carbonate rocks which contain appreciable amounts of shale. It was shown by Patnode and Wylliel in 1949 that shaly rocks exhibit an abnormally low resistivity when saturated with solutions of low ionic concentrations. This phenomenon has been demonstrated to be due to the adsorptive properties of shale or clay in the rock.' In estimating the fluid content of shaly sands or carbonates from the electric log, it is desirable and sometimes necessary to correct for the abnormally low resistivity. A similar correction is likewise often necessary if attempts are made to estimate the porosity of a stratum from resistivity measurements. The correction may be made from data obtained on core samples and from information on salinity of interstitial water. Cores, however, are not always available. Moreover, even if cores are at hand, their examination is time-consuming. It would be most desirable, therefore, to make corrections of this nature from the log itself. Since both the abnormal resistivity and the potential' are consequences of the adsorption of ions on shale, it should be possible to utilize the potential curve to give better interpretation of resistivity data obtained in logging shaly materials. The work described in following sections was directed toward this end. THEORY Relation of Resistivity of Shaly Reservoir Rock to Adsorpttve Properties In discussing the effect which the presence of shale or clay exerts on the resistivity of a reservoir rock, it is convenient to make use of the resistivity factor.4,5 This quantity has been defined as the ratio of the resistivity of the rock when it is completely saturated with an electrolyte to the resistivity of the electrolyte itself. When the rock, such as a clean sand or carbonate, is free of shale the resistivity factor is virtually independent of the ionic concentration of the electrolyte used to saturate the sample, so that F = R0/Rw = constant for a clean rock . . (1) where F is the resistivity factor, R0 is the resistivity of the rock saturated with electrolyte, and Rw is the resistivity of the electrolyte. When the rock contains argillaceous material, the resistivity factor as defined above is no longer independent of the concentration of the electrolyte used to saturate the rock, but decreases as the ionic concentration of the electrolyte decreases. In explanation of this behavior, it is instructive to consider a sample of shaly porous rock placed in contact with a large volume of a dilute electrolyte. The sample is considered to become saturated with the electrolyte, and to attain equilibrium with it. As a result of adsorption by the shale surfaces within the rock, there is a greater concentration of ions in the solution adjacent to the shale particles in the interstices of the sample than there is in the external solution with which the

Jan 1, 1955

By J. J. Oberly

WHILE examining lineage boundaries in germanium single crystals as described by Vogel et al.,&apos; patterns of conical etch pits were noted which reveal interesting properties of dislocations. The crystals were grown by pulling in the <100> direction, and (100) surfaces perpendicular to the growth direction were etched 4 min in a mixture of 6 cu cm HF, 10 cu cm HNO3, 6 cu cm acetic acid, 3 drops Br,. Lineage boundaries extended in any direction, but favored the <110> direction. The patterns which were noted first were composed of two or three etch pits arranged symmetrically about the lineage boundary, so that the doublets were spaced equally on either side of the boundary line and the triplets had their center pit on the boundary line. The triplets occurred less often than did the doublets; occasionally combinations were found. Two such combination patterns are shown in Figs. 1 and 2. The orientation of the patterns was determined approximately by subsequently etching the same surfaces in a mixture of 5 cu cm HF, 5 cu cm super-0x01, and 20 cu cm distilled water which produced nearby random square etch pits having edges in the <110> direction. In all cases, the axis of symmetry was <110>, being parallel to the etch-pit edges. Several successive lapping and etching operations showed that the patterns tended to continue through the crystal in the <100> direction, but eventually changed or vanished. It can be seen in both photographs that the pits in the patterns are much further apart than the pits in the adjacent section of the lineage boundary. In Fig. 1, the 10 pits of the pat-

Jan 1, 1955

By W. L. Ott, J. E. Hawley, C. L. Lewis

"IntroductionTHE APPLICATION of spectrochemical analysis to metals of the platinum group was advocated by Harvey (3) as follows: ""The spectra of the platinum group metals have been studied less than many of the more common metals. The rarity of occurrence of these elements makes the analysis relatively unusual. Potentially, the analysis of this group is an excellent application of spectrographic methods, particularly in contrast to the tedious chemical procedure"".Wichers (8) divides platinum-metal analysis into three broad divisions as follows :( 1) The detection and estimation of these metals in other materials, e.g., ores, where the amounts present are very small.(2) The detection and estimation of impurities in the refined metals themselves ....(3) The analysis of alloys of the platinum metals .....The present paper deals with the second division: analysis of refined rhodium.Research on spectrochemical techniques for determination of trace contaminants in refined platinum metals was begun at Queen's University in 1949, under the supervision of Professor J. E. Hawley. Since 1953, the work has been continued in the Metallurgical Laboratories of Falconbridge Nickel Mines, Limited. Techniques for spectrochemical analysis of refined platinum and palladium have been published ( 4, 5). A technique for analysis of refined iridium has been developed but not yet published."

Jan 1, 1955

By T. L. Joseph, G. Bitsianes

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

Jan 1, 1955

By E. R. Palowitch

Coal wasted with mine refuse represents losses in overall recovery of merchantable coal to the mine operator and a concomitant reduction in domestic reserves of available coal. Fraser, Kelley, and Graham3/ in studying the available coal in mine refuse in the Pittsburgh district of western Pennsylvania have estimated that at least 1 ton of mine refuse is produced for each 10 tons of merchantable coal and that 20 percent of this mine refuse might be recovered as salable coal by mechanical cleaning. SUMMARY This investigation dealt with the mechanical recovery of coal from wine refuse by a dense-medium washery employing pulverized mine rock as the dense medium and operating at a rate of 175 tons per hour. Two types of mint refuse were tested: Freshly mined and that .which had been mined 2 years before and piled on a waste dump.

Jan 1, 1955

By W. D. Mcmillan

Important reserves of nickel ore occur in the Levies district in Oriente, Cuba. The area is mountainous and mostly covered by heavy vegetation. The ore bodies comprise surface tracts of nickeliferous laterite underlain with decomposed serpentine of ore grade. The Cuban Nickel Co., a wholly owned United States Government corporation, owns a plant for leaching the nickel from its ores at Nicaro, Oriente, Cuba, Between December 1943 and March 31, 1954, 5,902,225 short tons of ore was treated, with a recovery of 116,206,519 pounds of nickel (52,711 metric tons). In 1953, 1,330, 224 short tons of ore was mined and 27;"3,129 pounds of nickel produced. The Cuban Nickel Co. also owns a townsite, with the necessary facilities, mining equipment, and 11 miles of railroad. Ore for the plant has been produced from the Ocujal-San Juan claims on lends owned by the Nicaro Nickel Co., a sub¬sidiary of Freeport Sulphur Co. The Government enterprise is man-aged by the Nickel Processing Corp. The Cuban Nickel Co. has denounced mineral concessions and has purchased other claims from private owners.

Jan 1, 1955

By Perry G. Cotter

As a portion of a general program for the synthesis of hard materials, a method was sought by which the hardness and density of tungsten carbide (WC)-cobalt compacts could be increased. It was demonstrated by Cotter that these improvements in quality could be made by employing an electric-resistance sintering process in which heat and pressure are applied simultaneously to presintered compacts composed of powdered tungsten carbide and cobalt. This conclusion was based on tests of material prepared by Cotter on welding equipment in use at the U. S. Naval Engineering Experiment Station, Annapolis, Md., and at Rensselaer Polytechnic Institute, Troy, N. Y. Rockwell-hardness tests made at Norris and core-drilling tests made at the Mount Weather Station of the Bureau of Mines indicated that, for some purposes, carbide material made by this process might be superior to the chemically analogous commercial products prepared by ordinary sintering methods. A program to develop optimum conditions for the electric-resistance sintering of tungsten carbide-cobalt compacts was initiated. The program was followed by a systematic evaluation of the hardness and density of compacts prepared by this method along with a series of carbide compacts furnished by various manufacturers. This paper presents a description of the electric-resistance sintering of tungsten carbide-cobalt compacts and the results of comparative physical tests.

Jan 1, 1955

By Harvey T. Kennedy, Erasmo T. Guerrero

In this investigation, the effects of the surface tension of brine and the interfacial tension between oil and brine on the recovery of oil by water flooding of Woodbine sand were studied. Variation of the surface forces was obtained by the addition of small amounts of commercially available chemicals, which did not appreciably change the surface tension of the oil. Fourteen surface-active agents, which were found to be effective in lowering the surface and interfacial tensions, were further investigated to determine the extent of their adsorption by the Woodbine Sand cores. It was found that adsorption was sufficient in all cases to prevent any substantial concentration of chemical at the flood front. The flow system was, therefore, brought to equilibrium with definite concentrations in the flood water by circulation before each test. The data thus have no relation to the results obtainable by using the chemicals in full-scale water floods, but should be helpful in predicting the performance of surface-active chemicals which are not lost by adsorption, if such can be found. Flow tests were made on various concentrations 01 six chemicals selected from the 14 investigated for surface activity and adsorption, with and without the presence of gas in the core. It was found that lowering the interfacial tension had a tendency toward reducing the recovery of oil and that the reduction of the surface tension of the brine had little or no effect. A substantial beneficial effect, however, resulted from the presence of gas in the cores. INTRODUCTION The movement and distribution of crude oil in a porous medium are governed by such factors as surfacc and interfacial tensions, viscosity of the oil, pore size configuration, and wetting characteristics of the medium. The knowledge of the part played by each of these factors is limited. If the oil is assumed to be distributed in droplets whose movement is restricted only by the pore openings, the following equation may be applied: ?P= 2r(1/r1-1/r2) .......(1) In this equation ?P is the pressure drop necessary to force an oil droplet through the construction, r is the oil-brine interfacial tension, r1 is the radius of curvature at the forward and smaller end of the deformed droplet, and r2 is the larger radius. This equation neglects the effects of viscosity, as a static or near static condition is assumed. It would apply equally well for a bubble of gas in liquid if r were taken as the surface tension of the liquid. This relation shows that droplets can be more easily displaced if the interfacial tension is decreased. The displacement of oil from the surface of a sand particle may also be considered from the basis of selective wetting assuming that the oil droplets are smaller than the pore constructions and that the sand surfaces may be considered as planes. A relation of the forces involved can be derived from Dupre&apos;s equation to give: Wos = row (1 +Cos?)........(2) where Wos = Work of adhesion between the sand and the oil row = Oil-water interfacial tension 0 = Contact angle ros = Oil-solid interfacial tension This equation would indicate that the displacement of oil from a sand surface is more readily obtained when the water-oil interfacial tension is reduced provided the contact angle remains constant. Evidently. however, the values of Cos 0 may vary along with the water-oil interfacial tension due to changes in the other surfaces of the system. The above theoretical considerations suggest that perhaps even the static behavior of a dispersed oil phase in a porous medium is considerably more complex than may be inferred by the simple systems

Jan 1, 1955

By W. O. Philbrook, K. M. Goldman, G. Derge

THIS is the third in a series of papers from the Metals Research Laboratory dealing with the transfer of sulphur across the iron-slag interface in a carbon-saturated system. The first paper&apos; showed that the transfer obeyed first-order kinetics. The second&apos; presented detailed evidence in support of the three-stage mechanism: FeS(Fe) FeS(slag) FeS(slag) + CaO(sing) ? CaS(slag) + FeO(slag) FeO(slag) + C ? Fe + CO. This emphasized the role of an iron-sulphur complex as the transfer agent across the interface and as an essential intermediate in the overall process. The present paper shows the influence on the process of the individual elements, carbon, silicon, manganese, and phosphorus, the alloying elements normally present and of interest in commercial blast furnace operations, aluminum, which has a pronounced accelerating influence, and nickel and copper, which are common minor impurities in the raw materials. The experimental methods and procedures for interpretation of data are the same as described earlier.1,2 Induction heated, graphite crucibles were used, and sulphur-free slag was added to the molten iron containing sulphur and the selected alloy. Slag samples were taken at regular time intervals and analyzed for sulphur and other components of interest. The authors wish to state specifically that these experiments were not intended to simulate industrial blast furnace operations. However, they do represent a study of the kinetics and mechanism of sulphur transfer at the slag-metal interface under specified laboratory control of the major variables in the system. It is believed that the results can be usefully applied to the blast furnace if consideration is given to the differences which are known to exist between the two conditions. A rigorous evaluation of the accuracy of rate studies is difficult. Recognized sources of error include sampling and analysis of both slag and metal, temperature measurement and control, selection of zero time, composition of the gaseous atmosphere over the reaction system, and extraneous sources of sulphur from the graphite crucible and reagent materials. In this study carefully standardized procedures were followed consistently in order to minimize the errors. It is believed that the reproducibil-ity of duplicate runs indicates that errors have been rendered negligible relative to the observed effects from intentional variables. For example, original experimental points for duplicate runs are shown in Figs. 1, 2, 7, etc. In most cases in this paper the drawn curves represent an average of at least two heats. The spread in sulphur values at a given time ranges from 0.02 to 0.08 pct, which is a small frac-tioi of the total values ranging up to 2 pct S in slag. In the systematic study of the influence of alloy additions, each element was added over a range of concentrations. The two slags used in this study were designated as "acid" or 1530 and "basic" or 1545. They had the nominal compositions given in Table I. Rates were measured in the temperature range 1500" to 1650°C. Data will now be presented to illustrate the various features of the study. Silicon The first alloying element examined was silicon, because its presence is unavoidable in any silicate slag system through the reaction y/2SiO2(slag) + xM?y/2Si(liq.Fe) + MxOy where M is any reducing agent such as iron or carbon. It is known that the attainment of equilibrium by this reaction is extremely slow and probably not reached in the blast furnace." The influence of silicon on the final stages of the sulphur reaction has also been studied.&apos; It has been shown5 hat silicon increases the activity of sulphur in iron. For such reasons silicon may also be expected to influence the kinetics of the reaction. The observed effects will now be described. The general procedure was to melt 530 grams of ingot iron in a graphite crucible, 3 in. OD, 2 1/4 in.

Jan 1, 1955

By R. V. Smith, E. J. Dewees, R. H. Williams

Before this paper was presented, the terms "f" and "v1/f in flow equations had been called "friction coefficient" and "friction factor," respectively. However, many authors have used the names for the terms interchangeably, with the result that considerable confusion has existed in the literature on flow of fluids. In an effort to establish a clear and concise terminology for these terms, the authors have designated f as "resistance coefficient" and dm as "transmission factor." Transmission factors for the flow strings of gas wells were determined by tests on wells in six fields of Oklahoma, Texas, and Louisiana. Data were collected on 14 gas wells while gas was flowing through 1 1/4, 2, 21/2, and 3-in. tubing and 51/2 and 7-in. casing. The transmission factors developed from these data were found to follow the resistance equation published by Nikuradse1 for turbulent flow in "rough" pipes with an average absolute roughness of 0.000,65 in. This average absolute roughness is believed to be representative generally of the flow strings of gas wells with the exception of those that have been exposed to corrosion or other conditions causing undue roughness. Also, use of an absolute roughness of 0.000,65 in. probably will result in transmission factors that are more representative of gas-well conditions than those in common use today, provided that the transmission factors are calculated by the methods outlined in this report. The authors believe that use of these transmission factors will permit calculation of more accurate subsurface pressures in gas wells than those in use today. Engineers use transmission factors in flow equations to compute subsurface pressures in flowing gas wells from measured wellhead pressures. These subsurface pressures are necessary for determining the productivity of gas wells from "back-pressure" tests. The methods of calculating pressures in flowing gas wells, as outlined by Rawlins and Schellhardt2 in Bureau of Mines Monograph 7, are based on the transmission factors in the well-known Weymouth formula" Natural gas engineers have realized that errors introduced by using transmission factors as given by the Weymouth formula are relatively unimportant in testing low-capacity gas wells; but they also know that such factors are important considerations in testing large-capacity wells. Accordingly, the research described in this report was undertaken to fulfill the need for more accurate means of calculating subsurface pressures in gas wells. This report is part of the Bureau&apos;s study of the flow of natural gas through pipe and commercial pipelines. Several of the conclusions regarding flow in the flow strings of gas wells were influenced by the results of the study of flow in horizontal pipelines. These instances are mentioned in the text of this report. METHODS OF COMPUTING TRANSMISSION FACTORS Methods and procedures for computing transmission factors for turbulent flow in circular pipes from test data taken on gas wells have been derived and explained in detail in a paper by Smith4. As these methods were used to calculate the transmission factors presented in this report, a summary is included. Starting with

Jan 1, 1955

By J. G. Kirby

The number of petroleum refineries in the United States continued to decline during 1954, and according to the Bureau of Mines annual survey there were 326 refineries with a total daily throughput capacity of 8,420,630 barrels, as of January 1, 1955. The increase in capacity for the year was 413,733 barrels daily, while the number of refineries declined 11. The capacity of the average refinery to process crude oil increased during 1954 from 23,759 barrels daily to 25,830. Breaking down the crude-oil capacity increase, by refining districts; 32 percent was installed at refin¬eries located in the Texas Gulf Coast district, 25 percent in the East Coast district, and 13 percent in both the Louisiana Gulf Coast and the California districts. The Appalachian No. 1, Texas Inland, and New Mexico refining districts reported declines in capacity during the year. Additional crude-oil capacity under construction, January 1, 1955, totaled 146,800 barrels daily. Included in this total are 4 new refineries, 1 each in California, Minnesota, New Mexico, and Washington. In addition to the&apos; new facilities, equipment producing 1.49,550 barrels daily is being replaced.

Jan 1, 1955

By B. W. Gandrud

At the Southern Experiment Station of the Federal Bureau of Mines, reports are prepared from time to time on results of washability studies of commercially important coal beds in the Southern Appalachian region. The investigations that provide the material for these reports are made by the Bureau of Mines, United States Department of the Interior, in cooperation with the University of Alabama and the mine operators. This report records the results obtained on a sample of run-of-mine coal taken in June 1953 from the Pratt bed at the Davidson Coal Co. mine about 1 mile west of Graysville, Ala. One of the main objectives of a washability study is to obtain technically and commercially important data in connection with the best methods for preparing and utilizing the Nation&apos;s limited reserves of good coking coal. Such information is important from the standpoint of conservation in that it facilitates selection of preparation methods that will yield an acceptable grade of coking coal with a mini-mum of losses of coal in the rejects. The Pratt bed is one of the main sources of coking coal in the Jefferson County part of the Warrior field. This is the first time, however, that data from a complete washability study of coal have been obtained from this bed in Jefferson County. In the Graysville area, Pratt-bed coal has good coking characteristics and is used for blending with other coals in making metallurgical coal. The extent of its use in such blends is severely limited in this area, however, by the fact that it has a high sulfur content, which has not been reducible to any great extent by washery treatment.

Jan 1, 1955