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By P. Bardzil, J. Gurland

An experimental study of the variation of transverse-rupture strength with composition Anexperimentaland grain studysize has shown that the strength reaches a maximum for values of the mean free path between carbide particles of 0.3 to 0.6 microns. The fracture oforiginates in and proceeds through the carbide grains mainly. Impact strength and hardness also were recorded. MOST of the physical properties of sintered carbides vary linearly with composition. The transverse-rupture strength, however, shows a unique behavior. As the amount of binder metal is varied from 6 to 25 pct by weight, the strength at first increases; then, between 15 and 20 pct Co, it reaches a maximum of nearly 400,000 psi, and finally decreases with further additions of binder metal. This behavior of the transverse-rupture strength has been reported, among others, by Englel and Sandford and Trent.' The significance of these observations has not been discussed in the literature. That it may be of more than specific importance is indicated by the very similar variation of strength with composition encountered in other systems sintered in the presence of a liquid phase, such as Tic-Ni3 and Fe-Cu.' Experimental Details All compacts were prepared and sintered according to normal industrial practice. The average diameter of WC grains and the mean free path between grains were measured on metallographically prepared samples by a method of linear and planar analysis sing the relations where d is the average diameter of dispersed grains; Nl is the number of noncontiguous grains intersected on a metallographic plane by a line of unit length; N, is the number of noncontiguous grains per unit area; P is the mean free path between grains of dispersed phase; and f is the volume fraction of dispersed phase. Approximately 1000 grains were counted on each sample. For each composition d2 was plotted against P, the resulting straight lines serving as a check on the measurements. The distribution curves of the WC powders of different average diameters were homologous, and no attempt was made to influence the grain size by blending powders, adjusting the sintering conditions, or otherwise altering the particle size distribution. Densities were measured by differential weighings in air and water. The degree of densification did not vary consistently with either composition or grain size. The density is influenced by slight amounts of impurities, specifically by 0.1 to 0.2 pct Fe which enters the powders during ball milling. As an illus- -tration of the experimental variations, a number of measured densities are listed in Table I. They are expressed in percentage of theoretical density, as calculated from the published X-ray densities of WC and Co.' For the purpose of determining the transverse-rupture strength, rectangular test specimens (3/16x 3/8x3/4 in.) were broken by loading at the center of a 9/16 in. span. The average strength of five or more samples is reported for each composition and grain size. The compacts were ground on two parallel surfaces only. The load was applied at an average rate of 6,800 psi per sec. Since the elongation after fracture of the alloys is very small, it was assumed that the compacts deform elastically to failure and the fracture stress was calculated by the conventional beam formula. The data for one alloy are presented in Table II as an example of the results and scattering ranges encountered. The precision of the test, as measured by the average difference between duplicates, is of the order of 15,000 psi. The results are strictly comparable only to compacts prepared and tested in the manner described and of similar chemical composition and grain size characteristics. Unnotched Charpy specimens were used for impact testing. Each point represents the average of 3 to 20 samples, the larger number being used in an attempt to determine the influence of grain size. Considerable scatter was encountered, the range from lowest to highest value often amounting to 30 pct of the impact strength. The hardness is reported as a Ra reading, using a 60 kg load with diamond brale indenter. Compositions are given in weight percent.

Jan 1, 1956

By J. B. Campbell, V. V. Valleroy, B. T. Willman, L. W. Powers

A steam drive of heavy oil was field tested in a shallow, low oil-saturation formation near Deerfield, Mo. The pilot was conducted in the Warner formation, a sandstone containing an 18' API oil having 1,000-cp viscosity at the 60F origind reservoir temperature. The formation war at a depth of 160 ft. Steam was injected into nine input wells arranged in an array of inverted five-spot patterns. In the completely confined center pattern, 14 temperature observation wells were installed to obtain thermal data and observe test progress. Late in the test, slugs of ammonia were injected to trace the flow paths of injected fluids. From the test area about 7,000 bbl of oil were produced. Data were obtained on areal and vertical temperature distribution, steam front advance, reservoir fluid movement and terminal saturations. This field test of a steam drive (I) demonstrated the feasibility of the method, (2) confirmed that the low residual oil saturations observed in the laboratory are obtained in the steam-swept region in the field and (3) provided recovery and conformance data for one set of field conditions. INTRODUCTION The Deerfield steam drive pilot test was conducted in a shallow sandstone containing 1,000-cp oil. The venture was undertaken cooperatively by the research and production departments of Carter Oil Co., which organizations have since been consolidated into Esso Production Research Co. and Humble Oil & Refining Co.. respectively. The production department was interested in steam injection at Deerfield because it appeared to be the most promising method of commercially producing this heavy oil deposit. The research department was interested in applying the new recovery method and in evaluating its performance in the field. At the time the test was begun, the initial oil saturation was not well known. Subsequent air coring and early pilot results confirmed that there was too little oil in place for profitable commercial exploitation by steam. Pilot termination at that time, however, would have been premature for evaluating field performance of the process, and the tert was continued to obtain additional data on steam injection as a recovery method. The test was located in Vernon County, Mo., about 10 miles north of the town of Deerfield and only a few miles from the Kansas border. The pilot site was selected as typical of the area. The location represented neither the highest nor the lowest oil saturation region in the acreage under lease in 1954. The steam drive was conducted in the Warner sandstone of Lower Pennsylvanian age. At the test site the top of the Warner occurs at about 160 ft subsurface and the formation is a fine- to medium-grained micaceous sandstone that dips gently to the northwest at the rate of 12 to 15 ft/ mile. A cross-section and permeability profile of the test location are shown in Fig. 1. At the pilot location the average total thickness of the Warner formation is about 43 ft, but the effective thickness for steam drive is 26 ft. Two distinct types of hydrocarbon saturation are apparent. The lower portion of the total sand, averaging about 17 ft thick, contains a very heavy asphaltic material that will not flow under the influence of a steam drive. This bottom interval, referred to as a dead oil residue, was not considered as part of the net sand undergoing steam exploitation. The initial formation and fluid properties of the upper 26 ft in the test area are summarized in Table 1, and variation of oil viscosity with temperature is shown in Fig. 2. Imbibition tests on preserved core samples taken at the end of the pilot test showed that the Warner sandstone was then neutral or slightly water-wet. Initially, the reservoir may have been strongly water-wet as indicated by low relative permeability to water during both water injection testing and early steam injection. PRIOR HISTORY Initial production tests of wells at the pilot site produced water with only a faint show of oil. No gas was produced except at Well 7-W in the pilot area and at another well about 1/3 mile northeast of the pilot. Prior to the start of the steam drive, a two-well water injection test and a two-well air injection test were conducted. No oil was produced by either. Water was pumped into Well I-W in the northeast corner of the pilot area with simultaneous production from Well 1 (Fig. 3). The air-injection tat was run at input Well 9-W and its offset, Well 2, in the southwest corner. Air and water injectivities were about the same when corrected for viscosity and pressure differences.

G. A. Burr, Parral, Chihuahua, Mexico (communication to the Secretaryt): I regret that Mr. Norris did not give more attention to the hoisting of water in inclined shafts or slopes: the only slope mentioned being Hickory Ridge Slope, No. 4, of the Union Coal Co. The surface arrangement, illustrated in Fig. 12 of his paper, if not unpractical, is at least unscientific and cumbersome. It is my opinion that the back- and sideguides shown in Fig. 12 are not only unnecessary where rails are used as a track, but are unsafe, excepting in the case of a very firm hanging-wall, or roof, and sides of vein-matter, having absolutely no tendency, either to settle from the back, or to squeeze from the sides, an effect which would inevitably force the guides out of alignment. The accompanying illustration, Fig. 1, shows what I consider a better method of hoisting water than that described by Mr. Norris. This method is based on the general practice in metalliferous mines of the West, where skips are used in slopes; and, while it is not original with me, I have frequently used it with very satisfactory results for dumping both ore and water.

Jan 1, 1904

By Dwight L. Baker, Alexander Knoll

The work herein reported shows that galena in certain organic solutions of fatty acids becomes coated with lead soaps, and that this coating is not only highly water-repellent but is also repellent to certain organic liquids, particularly those of high surface tension; i.e., nitrobenzene, diphenylmethane. Wetting Properties of Galena in Nonaqueous Fatty Acid Solutions When a "captive bubble"I is withdrawn from a polished, plane galena surface under a nitrobenzene solution of stearic acid, the air bubble shows a decided tendency to "cling" to the mineral surface. The contact angle, therefore, was greater than zero, although it was not large enough to be measured quantitatively by the captive-bubble method." When pure nitrobenzene was substituted for the nitrobenzene-stearic acid solution, no clinging of the bubble was observed; viz., contact angle = zero. Although the contact angle developed in air-galena-nitrobenzene-fatty acid solution was small, the organic solvent repellency of the galena surface was great enough to enable good recovery in a laboratory flotation cell2 In Table I are given the results of flotation experiments using several different fatty acids dissolved in nitrobenzene.

Jan 1, 1943

By Alexander Knoll, Dwight L. Baker

The work herein reported shows that galena in certain organic solutions of fatty acids becomes coated with lead soaps, and that this coating is not only highly water-repellent but is also repellent to certain organic liquids, particularly those of high surface tension; i.e., nitrobenzene, diphenylmethane. Wetting Properties of Galena in Nonaqueous Fatty Acid Solutions When a "captive bubble"I is withdrawn from a polished, plane galena surface under a nitrobenzene solution of stearic acid, the air bubble shows a decided tendency to "cling" to the mineral surface. The contact angle, therefore, was greater than zero, although it was not large enough to be measured quantitatively by the captive-bubble method." When pure nitrobenzene was substituted for the nitrobenzene-stearic acid solution, no clinging of the bubble was observed; viz., contact angle = zero. Although the contact angle developed in air-galena-nitrobenzene-fatty acid solution was small, the organic solvent repellency of the galena surface was great enough to enable good recovery in a laboratory flotation cell2 In Table I are given the results of flotation experiments using several different fatty acids dissolved in nitrobenzene.

Jan 1, 1943

By E. P. Fleming

COMPARED to the situation abroad, the domestic industry continues to lag both as regards the production and consumption of newly mined lead. During 1938 we produced and consumed slightly over 20 per cent of the world output, whereas ten years ago the figure was nearly double this pro- portion. Labor difficulties and absence of demand were chiefly responsible for the general inactivity. In the foreign field, in spite of low metal prices, production and consumption of lead equaled or exceeded all previous records. Practically all the large companies, with the exception of those in Spain, increased operations, though it should be noted that the foreign lead mines have higher-grade ores than domestic mines. In view of the rapid expansion of the foreign industry, it is natural to expect greater progress abroad, particularly in process metallurgy.

Jan 1, 1939

By W. T. Isbell

Although the pressure to meet the heavy demand for lead still took precedence over new metallurgical developments in the field of roasting, smelting, and refining of lead in 1948 there nevertheless has been considerable activity in the experimental development of new processes and improvements as well as plans for the modernization of many plants both here and abroad. Increasing labor and material costs have stimulated the trend to greater mechanization, revamping of flow sheets, and construction of larger units wherever possible. Although there have been many serious labor stoppages in the United States, Mexico, and Europe, labor supply has improved in most plants even if it has fallen off in efficiency.

Jan 1, 1949

By A. E. Gorum, I. Cornet

Fatigrle of ionic crystals has been studied primarily in magnesinm oxide. under cyclic stress dislocations move irrreversibly; they multiply; slip bands form and grow; cracks mucleate and propagnte, and failure occurs. The use of ionic crystals such as MgO is advantageorus in such investigations because they are optically transparent. Individual dislocation Intersections with {100} surfaces may be observed with a standard microscope, using etch-pit techniques. Slip, deformation, crack .formation, and fracture in MgO crystals under cyclic stress are compared with cotrresponditzg processes in metals. ThE effect of cyclic loading in metals has been studied for many years. The appearance of slip lines is readily observed and the ensuing fracture may also be seen. From these observations it is possible to predict the behavior of a material and make an educated guess as to what is happening internally, but the actual changes taking place within the structure are not readily apparent. If one could obtain a material in which the individual glide components could be observed, it would be invaluable in determining the actual slip distribution resulting from cyclic loading as well as the distribution of slip in the neighborhood of a growing crack. Such a material is magnesium oxide. Dislocation arrays may be observed by means of etch pits

Jan 1, 1961

By D. R. THOMAS

GENERALLY speaking, the production of other metals in Mexico fluctuates with that of silver. The first commercial discovery of mineral was in Taxco, Guerrero, in 1552. Five years later, the patio process was introduced at Pachuca, by Bartolome de Medina. In 1884, the main line of the Mexican Central R. R. was completed and a few years later, the National railway. In 1907, the patio process, after 350 years of successful operation, was replaced by cyanidation. Soon after the completion of the railroads, smelters were built at various points and provided means of treating ores that could not be treated by any of the processes existing at that time, such as patio, lixiviation, or pan amalgamation. As a result, a number of mines were developed along the railroads and even far \ out in the mountains. In order to facilitate the shipment of this ore to the smelters, purchasing agencies were established, which for a time were very profitable; most of these agencies are now permanently closed.

Jan 1, 1921

By Ernest R. Lilley

THOSE acquainted with the fundamental differences between the, educational .systems of Great Britain and. the United States would hardly expect .the training of men for the petroleum industry to proceed along the same lines- in the two countries. The youth entering an English university is, except in the case of-the student from some of the British colonies or from foreign countries, almost invariably a product of the English "public school." This is in no sense comparable .with the American public school. It is a private institution, frequently of considerable age and heavily endowed. In many aspects it seems to be comparable with the American preparatory school. Yet to some extent its activities remind one of the first years of the undergraduate: course in the American college. Certainly it takes to-itself many of the social, functions of the American college.

Jan 1, 1931

(The following list contains the names of those members of the Institute of whose connection with military service we have only recently become acquainted; it also includes the names of a few who have recently been promoted or transferred, indicated by a *. A complete list was published in the Year Book, issued as a supplement of the Bulletin for March, 1915.) ADAMS, ARTHUR K., Lieut., Co. 2, E. 0. T. S., Camp Humphreys, Va. AMIDON, CLAUDE E., 11th Training Co., Casual Camp, Camp Cody, N. M *BARBOUR, P. E., Capt., Engineer Corps, U. S. A. *BENHAM, W. M., Master Engr., Headquarters Dept., 115th Engrs. A. E. F., Care Postmaster, N. Y. BICKNELL, H. L., Pvt., Co. D, 27th Engrs., Camp Leach, D. C. *BLANDY, S. H. B., Lieut., Royal Horse Artillery, B. E. F.

Jan 10, 1918

H. A. BUEHLER, Rolla, Mo. -I consider the lead .and zinc deposits of the Mississippi Valley to be the result of descending waters. There are many features that we have not determined and yet when you see the general field relations, it seems to me that the cause and effect can be well explained by descending circulation. In the Joplin-Miami district, for instance, the ore deposits are connected with openings or with old cavity fillings which have a direct connection downward from the surface to practically 300 ft. In the Miami camp, in the western part of the field, some of the deepest orebodies are directly connected with water, channels; the same condition has been obvious and always present with the shallower ores. I speak of one deposit that I have examined more thoroughly than any other in that district, the Admiralty property, which contains large openings or caves at the deepest levels. It seems to me that waters which would pass upward through 1800 ft. of dolomite would be saturated with lime and magnesia so far as the carbon dioxide of those waters would dissolve them, and therefore, on

Jan 1, 1918

By W. S. Owen, T. Bell

The variation ox the M, temperature with nitrogen concentration has been determined experinzentally. The free-energy difference between martensite and the parent y Phase at the M, temperature,is computed for Fe-C and Fe-N alloys using recent solubility data fm the Fe-N system and new data for the variatim of the activity of the interstitial solute in the y phase with concentration. The "geometric model" is considered also, and the importance of Zener ordering is noted. It is shown that, although at any chosen concentration the M, temperature and the activity are significantly different in the two alloy systems, the free-energy duference is the same within the limits of experimental error, thus Providing further evidence of the very close similarity between the martensite transformations in Fe-C and Fe-N alloys. TO estimate the free-energy change accompanying the martensite transformation in binary interstitial alloys it is necessary to know the variation of the Ms temperature with interstitial solute concentration and some thermodynamic data. To date, only the Fe-C system has been discussed because this was the only system for which relevant experimental measurements had been made, but even in this case the data available are insufficient to permit the free-energy change to be calculated without the assumption of a thermodynamic model for the y and a solid solutions. The last comprehensive discussion of the topic was by Kaufman, Radcliffe, and Cohen in 1.960.' Since that time Ellis, Davidson, and Bodsworth2 have redeter mined the activity of carbon in y iron as a function of carbon content and Atkinson3 has measured the activity of nitrogen in Fe-N austenite. The M, temperature of Fe-N is reported in the present paper. Thus, it is now possible to assess the free-energy change accompanying the martensite transformation in Fe-N alloys on the same basis as that used to assess the change in Fe-C alloys. This comparison is of interest because it has been shown recently4 that the structure of the martensite formed in Fe-N alloys changes with nitrogen content in a manner exactly parallel to the changes in structure in the Fe-C series and that the strain associated with the distortion of the iron lattice in either the y or the a phase by a nitrogen atom is the same as that produced by a carbon atom. The work to be described tests whether or not this close similarity between the two systems extends to the thermodynamics of the martensitic transformations. THE Ms TEMPERATURES FOR Fe-N MARTENSITE Bose and Hawkes5 found the M, temperature of a eutectoid Fe-N alloy (2.35 wt pct N) to be 35°C. This single determination appears to be the only reported measurement of the M, temperature of an Fe-N alloy. In the present work a series of more than fifteen different specimens containing between 0 and 2.7 wt pct N were prepared by controlled nitriding of pure iron wire 0.010 in. diam. The iron was supplied by B.I.S.R.A. and was designated ACN2. The nitriding procedure, all aspects of which are critical, has been described in detail elsewhere.' Each specimen was quenched from the austenitizing temperature into brine at 20°C without removing the specimen from the ammonia-hydrogen atmosphere in which it was ni-trided. Alloys containing up to 0.7 wt pct N were fully martensitic. More concentrated alloys contained progressively more retained austenite. At 2.34 wt pct N the specimen was completely austenitic after quenching to 20°C. The M, temperature of specimens with M, temperature above 20°C (those containing less than 2.35 wt pct N) was determined by a thermal arrest technique. For the more concentrated alloys (2.35 to 2.70 wt pct N) the variation of electrical resistance with temperature down to -196°C was used. Unlike Fe-C alloys, Fe-N alloys cannot be reaus-tenitized in vacuum or in an inert atmosphere because excessive loss of nitrogen occurs, even in short times, at high temperatures. Consequently, the alloys were reaustenitized in the ammonia-hydrogen mixture corresponding to nitrogen equilibrium at the temperatures used. The specimens were quenched in a blast of cold hydrogen gas and the temperature, measured by a thermocouple welded to the 2.5-in.-long specimen, was recorded on a high-speed recorder. In the first experiments 0.002-in.-diam chromel-alumel wire thermocouples were used but it was found that these gave erroneous readings due to contamination by nitrogen pickup. Pt-Pt 13 pct Rh wires of 0.002 in. diam were found to be satisfactory. Further details of the experiments are available in the original thesis.7 The cooling rate was controlled between 400° and 4000°C per sec by adjusting the hydrogen pressure. At least three cooling curves were obtained for each composition. Each specimen was analyzed for nitrogen after quenching. To aid in the accurate location of the martensite arrest points a series of cooling curves of 0.010-in.-diam platinum wire were recorded and these, which did not contain an arrest, were used as comparison standards. Four specimens, each in the form of a 3-in. loop, were prepared from each of the four alloys containing more than 2.35 wt pct N. One specimen was used for nitrogen analysis, one for X-ray diffraction, and two for resistance measurements below 20°C. The latter specimens were quenched from 20°C into constant-temperature baths at selected lower temperatures.

Jan 1, 1968

Abbey, Robert Graham, District Mgr., The W. W. Sly Mfg. Co., 50 Church St., New York, N. Y. '21 Abbott, A. N Ave. Morelos 84, Cuernavaca, Morelos, Mexico '23 Abbott, Argyle Campbell, Geol 42 Everett St., Arlington, Mass. '29 Abbott, Clarence E., V.P., Charge of Raw Materials, Tenn. Coal, Iron & R. R. Co., 1242 Brown-Marx Bldg., Birmingham, Ala. '04 Abbott, Louis Benjamin, Chief Engr., Consolidation Coal Co., Watson Bldg., Fairmont, W. Va. '15 Abeel, George H., Jr., Cons. Min. Engr 1281/2 S. Canon Dr., Beverly Hills, Cal. '18 Abel, Raymond L., Asst. Prof., Dept. of Pet. Refin., Univ. of Pittsburgh. .Pittsburgh, Pa. '28 Abel, Walter D., Cons. Engr 650 S. Grand Ave., Los Angeles, Cal. '82 Abele, Louis T., Min. & Met. Engr., Supt., Texas Hill Mine Coulterville, Cal. '31 Abell, Leo M. Millicent, S. Australia '31 Abernathy, George Elmer, Prof. of Geol. & Min., Kansas State Teachers College, Pittsburg, Kan. '20 Aborn, Robert H., Research Lab., U. S. Steel Corp. Lincoln Highway, Kearny, N. J. '19 Abozeid, Mahmood, Dept. of Mines & Quarries Cairo, Egypt '26

Jan 1, 1932

By R. W. Cahn, C. D. Graham

The rate of growth of a single grain growing into a strained aluminum single crystal, measured by the conventional heat-cool-etch technique, is shown to decrease with time at temperature. The growth rate measured by means of X-rays, with the sample continuously at temperature, is found to be linear. Evidence is presented to show that the decreasing growth rate obtained by the conventional technique is due to abnormal recovery in the strained grain, and that the recovery in turn results from the heating and cooling cycles, rather than from the effects of etching. The experimental apparatus is described in an appendix. FREQUENTLY, the rate of grain boundary motion during recrystallization is determined by heating a sample to a known temperature for a given time, cooling to room temperature, and etching to reveal the boundary position. The cycle of operations is repeated as many times as necessary to establish the rate of boundary motion. Although this heat-cool-etch technique has been used by a number of workers over a period of many years,'-!' other investigators have encountered difficulty with the method."'. " They have attributed the erratic results to the effects of repeated heating and cooling, or of etching, or both, and have adopted an alternative experimental procedure in which a number of identical samples are employed, each sample being cooled and etched only once. This alternative method ove1.comes some difficulties, but introduces others. In particular, the incubation periods of the observed grains are unknown: any effect of crystal orientation on growth rate cannot be determined easily. A preferable method would be to measure the motion of a recrystallizing grain boundary with the sample at temperature without etching," but such measurements have in the past been restricted to nonmetals. This paper describes the construction and operation of a device, the goniometer furnace, with which the position of a moving grain boundary between a recrystallizing grain and the strained single crystal into which it grows can be measured by means of X-rays, with the sample maintained continuously at temperature. Goniometer Furnace The operating principle of the goniometer furnace is shown in Fig. 1. The sample, in the form of a bicrystal strip, is surrounded by a furnace, not shown in the sketch, and can be rotated about the two axes A and B which intersect at the point where the X-ray beam strikes the strip. The strip is oriented so that one of the two grains gives a strong Bragg reflection, which is detected by a suitably placed Geiger-Miiller counter coupled to a counting-rate meter When the strip is moved parallel to its own length in the furnace, arrow C, so that the X-ray beam strikes the second grain, there is in general no strong reflection. By noting the position of the strip at which the drop in Geiger counter reading occurs, it is possible to determine the position of the boundary. Measuring the change in boundary position with time at temperature gives the rate of growth of the recrystallizing grain. Details of the construction and operation of the goniometer furnace are given in the Appendix. Measurements showed that the temperature in the furnace was uniform within ±10°C over its working length of about 28 cm. The temperature at the measuring position, i.e., at the point where the X-ray beam struck the sample, was estimated to be constant within ±2oC. Using the goniometer furnace, the position of a stationary boundary could be measured with a reproducibility of ±0.3 mm. At elevated temperatures, 500" to 625"C, with the boundary in motion and the X-ray reflection less sharp, the estimated accuracy of each measured boundary position dropped to about ±1 mm. Experimental Results The test pieces were single crystals of 99.6 pet A1 —principal impurities 0.19 pet Fe and 0.12 pet Si— 1 mm by 1 cm in cross section and 6 to 10 cm in length, grown by the strain-anneal method. This relatively low purity material was used because of the difficulty encountered in producing strain-anneal single crystals of very high purity—99.996 pet—

Jan 1, 1957

By Charles A. Schffer

Several months ago, some specimens of the minerals occurring at the Etta tin mine, Dakota, were received at the laboratory of the Cornell University. On examining the heavy brownish-black portion, which I presumed was the tin-stone, I was surprised to find only a faint indication of tin. Further investigation showed the mineral to be tantalite. On searching carefully all the fragments received, a considerable quantity of that mineral was found, and only a single streak of cassiterite, which was attached to a mass of spodumene. Another lot of specimens, from the same locality, consisted of

Jan 1, 1885

By O&apos, R. G. Meara, B. W. Gandrud

In 1034 the Southern Experiment Station of the U.S. Bureau of Mines in cooperation with the University of Alabama began an investigation of the availability of kyanite ores as a source of raw material for the manufacture of refractories. Under this program, gravity concentration and flotation tests have been made on two varieties of Georgia kyariite ore, mica schist and massive. Most of the attention has been directed to the mica schist ores, as they are more widely distributed and seem to offer greater economic possibilities than the massive ores. It is evident that the preparation of kyanite for use as a refractory material involves other considerations than the mere elimination of impurities. A concentration process that eliminates impurities satisfactorily may have to be followed by some additional treatment, since the final product must be of a coarseness and size ratio that will make it suitable for refractories manufacture. So far in the investigation at the Southern Experiment Station of the U.S. Bureau of Mines only the concentration problem has been considered, and this paper is intended as an interim report. Ores The schist ores contain 1 to 9 per cent of kyanite crystals embedded in mica and quartz, with smaller amounts of graphite, garnet and iron oxide and minor amounts of other heavy minerals. The garnet content varies from a trace to a few per cent. The minerals are easily released by moderate grinding. The size of the kyanite ranges from fine needles to crystals 1 1/2 in. long, 1/2 in. wide and 1/4 in. thick. The garnet, quartz and iron oxide grains have a smaller mean mesh than most of the kyanite. The maximum size of the garnet crystals corresponds to about 14 mesh and that of the sand grains is considerably less. Most of the iron oxide is still finer, for the minus 100-mesh size is greatly enriched in Fe²O3. The massive ore consists of radiating masses of kyanite interlocked with quartz, mica, corundum and small amounts of other heavy minerals.

Jan 1, 1938

By B. W. Gandrud, R. G. Meara, O&apos

In 1034 the Southern Experiment Station of the U.S. Bureau of Mines in cooperation with the University of Alabama began an investigation of the availability of kyanite ores as a source of raw material for the manufacture of refractories. Under this program, gravity concentration and flotation tests have been made on two varieties of Georgia kyariite ore, mica schist and massive. Most of the attention has been directed to the mica schist ores, as they are more widely distributed and seem to offer greater economic possibilities than the massive ores. It is evident that the preparation of kyanite for use as a refractory material involves other considerations than the mere elimination of impurities. A concentration process that eliminates impurities satisfactorily may have to be followed by some additional treatment, since the final product must be of a coarseness and size ratio that will make it suitable for refractories manufacture. So far in the investigation at the Southern Experiment Station of the U.S. Bureau of Mines only the concentration problem has been considered, and this paper is intended as an interim report. Ores The schist ores contain 1 to 9 per cent of kyanite crystals embedded in mica and quartz, with smaller amounts of graphite, garnet and iron oxide and minor amounts of other heavy minerals. The garnet content varies from a trace to a few per cent. The minerals are easily released by moderate grinding. The size of the kyanite ranges from fine needles to crystals 1 1/2 in. long, 1/2 in. wide and 1/4 in. thick. The garnet, quartz and iron oxide grains have a smaller mean mesh than most of the kyanite. The maximum size of the garnet crystals corresponds to about 14 mesh and that of the sand grains is considerably less. Most of the iron oxide is still finer, for the minus 100-mesh size is greatly enriched in Fe²O3. The massive ore consists of radiating masses of kyanite interlocked with quartz, mica, corundum and small amounts of other heavy minerals.

Jan 1, 1938

By Brahm Prakash, R. Schuhmann

Chemical conditions for flotation and nonflotation of quartz with oleic acid as collector and barium, calcium, aluminum, iron, and tin as activators were studied using a simple vacuum-flotation technique in glass-stoppered graduates. The detailed study of barium activation led to an interpretation based on ideal Langmuirian chemi-sorption. FLOTATION of quartz is of practical importance as something to be avoided in soap-floating many types of ores. Clean, unactivated quartz is not floated with fatty acids and soaps, such as oleic acid and sodium oleate, in the quantities normally used for flotation. However, data in the literature indicate that almost any multivalent cation will activate quartz if given an opportunity. Thus, a common problem is to prevent activation of quartz by the various inorganic cations inevitably present in flotation pulps. Wark and his coworkers1 have demonstrated the reversibility of the chemical reactions and adsorptions involved in the activation, depression, and collection of the common sulphide minerals. The procedure in much of their work was to bring a mineral surface to equilibrium with solutions of known pH, collector concentration, and activator concentration, and then to test the floatability of the mineral by contact-angle measurement. From the data, graphs were constructed with pH and reagent concentrations as coordinates. These graphs show fields of flotation and fields of nonflotation, separated by narrow transition regions whose locations are shown by so-called contact curves. From the shapes and locations of the contact curves, which roughly separate fields of flotation from fields of nonflotation, a quantitative understanding of the interaction of the reagents with each other and with the minerals often can be deduced. The study of quartz flotation to be described in this paper follows in broad lines the approach of Wark and coworkers. That is, pH, activator concentration, and collector concentration were varied to find equilibrium conditions of flotation and non- flotation, and the results are presented graphically by means of contact curves. However, instead of testing for floatability by measuring the contact angle on a polished surface, a simple vacuum flotation technique was developed and used. Purified oleic acid was the collector and terpineol the frother. Barium activation was studied in some detail, and exploratory studies were made of activation with calcium, aluminum, ferric iron, and stannic tin. Preparation of Materials Quartz: Large lumps of high-grade vein quartz were crushed dry in a cone crusher and rolls. The —20, +28-mesh portion was screened out and used in the subsequent steps. This material was passed through a high-intensity magnetic separator to discard iron, then leached twice with hot concentrated HCl and washed repeatedly with distilled water. The cleaned sand was then wet ground with porcelain balls in a porcelain pebble mill, deslimed repeatedly by settling and decantation to discard —800-mesh material, and again washed with hot HCl followed by distilled water. The resulting stock of quartz was stored under water. Chemical analysis gave 99.8 pct SiO2. Table I gives the size analysis of the quartz used for flotation tests. Calculations from these data, using shape factors given by Gaudin and Hukki9 indicate a specific surface of about 500 cm2 per g. Blank flotation tests in distilled water, and in water with added frother, showed the prepared quartz to be completely nonfloatable and thus indicated the absence of organic contamination. Oleic Acid: The preparation of oleic acid was based on fractional vacuum distillation of methyl oleate2,3 followed by regeneration of oleic acid, and finally fractional crystallization of oleic acid from acetone solutions at low temperatures." The pure oleic acid was stored in a refrigerator. The iodine number of the oleic acid was found to be 90.0 (theoretical 89.93). Oleic acid was used in the form of a dilute water solution of sodium oleate, after preliminary flotation tests showed no effects of form of addition and order of addition of reagents when an adequate conditioning time (that is, 30 min) was provided. Other Reagents: Sodium hydroxide solutions low in carbonate were prepared by first making 1:1

Jan 1, 1951

By Brahm Prakash, R. Schuhmann

Chemical conditions for flotation and nonflotation of quartz with oleic acid as collector and barium, calcium, aluminum, iron, and tin as activators were studied using a simple vacuum-flotation technique in glass-stoppered graduates. The detailed study of barium activation led to an interpretation based on ideal Langmuirian chemi-sorption. FLOTATION of quartz is of practical importance as something to be avoided in soap-floating many types of ores. Clean, unactivated quartz is not floated with fatty acids and soaps, such as oleic acid and sodium oleate, in the quantities normally used for flotation. However, data in the literature indicate that almost any multivalent cation will activate quartz if given an opportunity. Thus, a common problem is to prevent activation of quartz by the various inorganic cations inevitably present in flotation pulps. Wark and his coworkers1 have demonstrated the reversibility of the chemical reactions and adsorptions involved in the activation, depression, and collection of the common sulphide minerals. The procedure in much of their work was to bring a mineral surface to equilibrium with solutions of known pH, collector concentration, and activator concentration, and then to test the floatability of the mineral by contact-angle measurement. From the data, graphs were constructed with pH and reagent concentrations as coordinates. These graphs show fields of flotation and fields of nonflotation, separated by narrow transition regions whose locations are shown by so-called contact curves. From the shapes and locations of the contact curves, which roughly separate fields of flotation from fields of nonflotation, a quantitative understanding of the interaction of the reagents with each other and with the minerals often can be deduced. The study of quartz flotation to be described in this paper follows in broad lines the approach of Wark and coworkers. That is, pH, activator concentration, and collector concentration were varied to find equilibrium conditions of flotation and non- flotation, and the results are presented graphically by means of contact curves. However, instead of testing for floatability by measuring the contact angle on a polished surface, a simple vacuum flotation technique was developed and used. Purified oleic acid was the collector and terpineol the frother. Barium activation was studied in some detail, and exploratory studies were made of activation with calcium, aluminum, ferric iron, and stannic tin. Preparation of Materials Quartz: Large lumps of high-grade vein quartz were crushed dry in a cone crusher and rolls. The —20, +28-mesh portion was screened out and used in the subsequent steps. This material was passed through a high-intensity magnetic separator to discard iron, then leached twice with hot concentrated HCl and washed repeatedly with distilled water. The cleaned sand was then wet ground with porcelain balls in a porcelain pebble mill, deslimed repeatedly by settling and decantation to discard —800-mesh material, and again washed with hot HCl followed by distilled water. The resulting stock of quartz was stored under water. Chemical analysis gave 99.8 pct SiO2. Table I gives the size analysis of the quartz used for flotation tests. Calculations from these data, using shape factors given by Gaudin and Hukki9 indicate a specific surface of about 500 cm2 per g. Blank flotation tests in distilled water, and in water with added frother, showed the prepared quartz to be completely nonfloatable and thus indicated the absence of organic contamination. Oleic Acid: The preparation of oleic acid was based on fractional vacuum distillation of methyl oleate2,3 followed by regeneration of oleic acid, and finally fractional crystallization of oleic acid from acetone solutions at low temperatures." The pure oleic acid was stored in a refrigerator. The iodine number of the oleic acid was found to be 90.0 (theoretical 89.93). Oleic acid was used in the form of a dilute water solution of sodium oleate, after preliminary flotation tests showed no effects of form of addition and order of addition of reagents when an adequate conditioning time (that is, 30 min) was provided. Other Reagents: Sodium hydroxide solutions low in carbonate were prepared by first making 1:1

Jan 1, 1951