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By AIME AIME

ALTHOUGH the present economic depression is felt in the petroleum industry, probably as much as in any other branch of American industry, the Petroleum Section of the Institute was well represented at the general sessions on Monday and at all of the seven division sessions on Tuesday, Wednesday and Thursday. The seven sessions of the Division were so arranged as not to conflict and thus permitted members to hear the programs of all sessions.* The first meeting of the Petroleum Division was held on Tuesday afternoon; a joint session on engineering research and production engineering. The following papers were presented:

Jan 1, 1931

By T. D. Thomas

CONTENTS PAGE T. D. Thomas-Misfires in Anthracite Coal Mines 3 W. H. Forbes-Misfires in Bituminous Coal Mines 12 A. W. Worthington-Misfires in Non-metallic Mining (Limestone) 18 Misfires in Anthracite Coal Mines BY T. D. THOMAS, * LANSFORD, PA. (New York Meeting, February, 1929) IN THIS paper, major attention is given to misfires in mines where electric multiple shot-firing is the system used. Misfires are sometimes caused by one action or condition and at other times by a combination of two or more. They may be divided into two classes: (1) those caused by workers in the mines, (2) mechanical or manufacturer's causes. The second cause will be discussed first.

Jan 1, 1929

By M. S. Smani, P. Blazy, J. M. Cases

Investigations on the beneficiation of sedimentary Moroccan phosphate ores are reported in four separate parts. The first discusses electrochemical phenomena at the solid-aqueous solution interface for minerals of the apatite group. In the second part, the electrochemical properties of the calcareous gangue associated with the phosphate ore are investigated. The flotation of calcite and phosphate oölites, using both anionic and cationic collectors, is discussed in the third part. It is shown that selective recovery could be obtained for precise concentrations of collectors and pH ranges. Results of work aimed at optimizing depression of phosphate oölites during inverse flotation of the carbonate gangue with sodium oleate are reported in Part 4.

Jan 1, 1976

CHARLES KIRCHHOFF, Chairman. ALBERT SAUVEUR, Vice-Chairman. A. A. STEVENSON, Vice- Chairman. HERBERT M. BOYLSTON, Secretary, Abbot Bldg., Cambridge, Mass. John Birkinbine, J. Esrey Johnson, Jr., Felix A: Vogel, William H. Blauvelt, William Kelly, Leonard Waldo, James Gayley, Richard Moldenke, William R. Walker, Henry D. Hibbard, Joseph W. Richards, William R. Webster. Henry M. Howe, E. Gybbon Spilsbury, Frederick W. Wood. Robert W. Hunt, A. A. Stevenson is appointed an additional Vice-Chairman of the Committee. He will serve as Acting Chairman during the absence abroad of Professor Sauveur. For the meeting of the Institute which is to be held in New York City, Oct. 16 and 17, 1913, the following papers are now assured

Jan 7, 1913

By T. Lane Carter

BEFORE describing the experience with the Chinese on the Rand and the work they have accomplished, it will be necessary, sary, first, to give a brief account of labor-conditions in the Transvaal since the war, and then to show how the necessity of importation of labor arose. As is well known, the Transvaal mines are run on the dual system of labor-that is, the rough work is done by colored laborers under the superintendence of white men. From the start of mining operations in South Africa there has been the cry of shortness of native labor, due in great measure to the failure of Kaffirs to work continuously in the mines. While he works, the Kaffir is a satisfactory laborer, but his period of service is short, averaging about nine months. People unacquainted with the Kaffir have maintained that, by offering a higher wage and better accommodation, better results would be obtained from the native workers, but an increased wage simply aggravates the trouble. The Kaffir's wants are few. While at work he spends little of his money, and before long has sufficient capital with which to buy wives and become a gentleman of leisure. Doubling the wage of the Kaffir means that he acquires a competency in half the time, so that his period of service is correspondingly reduced. In 1899, before the war, there was always a cry about the scarcity of Kaffir labor. The highest number of natives at work was in July and August, 1899, when nearly 100,000 were employed. At the outbreak of hostilities the Kaffirs were scattered far and near, many doing well during the war by working for the military authorities. On the, resumption of mining operations on the Rand a serious mistake was made. Based on past experience, it was argued that if the whole industry decided to start anew with

Sep 1, 1908

By Robert W. Hunt

I have frequently stated that while the chemical composition of steel is important, yet even greater importance is connected with the mechanical and heat treatment of the metal. During the past year I encountered such a positive example of that fact that I deem it worth putting upon record. A prominent railway system divided an order for open-hearth steel rails between two steel works, both of which are under the control of the same corporation; giving to one about 18,000 tons, and to the other 7,500 tons of the same section and to be made under the same specifications. The rolling results obtained in the two mills varied so widely that a study of the figures is intensely interesting and serves to illustrate the advantages obtained by carefu1 ingot casting, and, quite as pertinently, the possible benefits of careful subsequent heating and rolling with moderate reductions in the rolling process. The smaller order was rolled complete in four installments during the same months that the larger order was being made in six separate installments; but, to permit of exact comparisons, the totals of the four installments (completing the order with the mill which I will call A) are given with the totals of the first four installments of the larger order, made by the mill designated as B. These rolling results are: Mill A. Mill B. Number of rollings,............................................ 4 4 Total number of rails rolled................................ 18,278 27,832 Percentage of rails cut to short lengths because of flaws near ends, etc......................................... 0.7 7.6 Percentage of rails made second quality for flaws, etc. 0.9 6.3 Percentage of rails scrapped for flaws, etc............... 0.6 4.5 Percentage of rails scrapped for failure at drop test... none 3.4 It should be stated that the figures given above cover all the reasons for putting the rails in the classes stated, Thus a part of the percentage of rails cut to short lengths may have been

Jan 1, 1914

By W. A. Boyer

MINE hoisting ropes can be loaded to capacity only when the strength of each component is exactly known. Characteristic curves provide this information. When load and rate of acceleration are specified for an individual rope, the characteristic curve assumes a predetermined shape. The factor of safety, is the value drived by dividing the breaking strength of the rope by the total stress on the rope where it goes over the sheave wheel. Total stress is made up of the weight of skip and cage, weight of ore, weight of rope between sheave and rope clevise or attachment, friction load, and acceleration force. Bending stresses are neglected in this discussion, as sheaves and drum di- ameters are assumed to be large enough to reduce these stresses to a negligible value. Fig. 1 gives a family of characteristic curves for 13/8-in. improved plow steel hoisting ropes of 6 x 19 or 6x21 construction with hemp core. The curves will hold for all rope sizes of this specified quality when they are subjected to an acceleration rate of 1.608 ft per sec2. As acceleration rates of most deep shaft hoists are close to this value, this family of curves is presented as a standard. Deviation is slight for other rope sizes. Note that for 0, which is the most important, the deviation is within the width of the line on the graph. In a comparison of values for ropes of 5/8-in. and 21/4-in. diam the deviation ranges from a maximum 1.2 pct at 0 ft to 0.6 of 1 pct at 5000 ft. The value of 5.55 is the same for all ropes at 2500 ft. The tabulated columns to the left of the curves are values of total connected load for each size of rope from 5/8-in. to 21/4-in. diam inclusive. With each of these connected loads the safety factor characteristic curve for the rope will be as indicated.

Jan 1, 1957

By A. B. Stevens

IN the calculation of oil and gas reserves by volumetric methods, it is necessary to know the volume of the reservoir available for the storage of the oil or gas. To obtain this information, a number of methods for determining both total and effective porosity of reservoir rocks are used. For the determination of the total porosity, or the porosity that considers all of the pore spaces, connected and isolated, the Russell7,8,9 and the Melcher-Nutting1-6 methods are the best known and most- widely used in the petroleum industry. These methods have disadvantages in that they give the total porosity of the samples and in that the samples are reduced to grain size in the determination. In many sands there may be little or no difference between total and effective porosity but in other sands there may be considerable difference between the two. For the estimation of oil-and gas reserves the effective porosity of the reservoir rock always should be used. Of the methods that have been developed for the determination of the effective porosity of reservoir rocks, or the porosity that considers only those pore spaces that are connected, the best known are the so-called Boyle's law6,10-13, and the Washburn-Buntings.5,6,11 methods. The Wash-burn-Bunting method is probably the most widely used because it gives effective porosity, it is rapid, and the apparatus is inexpensive. This method employs a special porosimeter in which the core sample is placed in direct contact with mercury. This method has disadvantages in that, as a result of the high vacuum created in the pore spaces, mercury is drawn into the openings, making it impossible to use the sample for a check determination and also ruining the sample for any further test, such as permeability. The purpose of this paper is to describe an appa-ratus employing the same principle as the Washburn-Bunting method but so designed that the core sample does not come in contact with the mercury in the porosimeter.

Jan 1, 1939

By Frederick Burbridge

The Morning silver-lead-zinc mine of the Federal Mining & Smelting Co. is about 'two miles northwest of Mullan, Ida. The lode is a metasomatic fissure vein. The orebody is approximately 2000 ft. long within the bounds of the property and varies in width from knife edge stringers to 50 ft. It has been developed to a depth of 3600 ft. and stands nearly vertical in Revett quartzite, which .strikes north 65" west. The high-grade veins and lenses are generally mixed with waste (siderite, quartz, and quartzite). The average grade of ore to sorting plant in 1921 was 4 oz. silver per ton, 8.6 per cent. lead, and 4.1 per cent. zinc. Wall rock stands only a short time without timbering. The minimum angle of gravity flow is 45". The ratio of waste sorted out to ore is 6 per cent. No gases are generated underground and temperature has no influence on mining operations. Fresh air is forced down the air raise and up the main shaft. Drifting and Stoping Main drifts 12 ft. wide and 13 ft. high are driven every 200 ft. (vertically) and are connected by raises 125 ft. apart. These raises consist of three compartments (chute, tramway, and timber slide) and are for the purpose of ventilation, access, and hoisting supplies to stopes. Ground is stoped between raises. Chutes are placed every 25 ft. for drawing off ore broken in stopes. Waste for filling is obtained from waste raises off the stope in walls or waste is dumped from the level above down the chute compartment of raises, which is bulkheaded so that waste can be drawn off at any floor as required. Timbering Posts and caps for square sets (varying in diameter from 6 to 24 in.) are cut to length in a sawmill on the surface. No preseratives are used. Timber is taken on a flat car along drifts to a raise nearest the working place and hoisted as required. Practically no timber is salvaged for

Jan 1, 1925

By H. I. Young

INASMUCH as there has been a great deal of activity in this district recently, a paper of this kind should treat of all the various phases of mining, namely, prospecting, developing and operating. PROSPECTING Where ore is found it a depth of 100 ft. (30 m.) or more, the prospect work is done by churn drilling. Several makes of churn drills are used in this work, both steam- and gasoline-driven machines being used. The drilling is usually started with a 6-in. bit, and the size of the bit is reduced, if necessary, as the hole is advanced. It is general practice to drill from 100 to 400-ft. holes, but this is governed entirely by the location and formation of the ground. In drilling sheet ground, close spacing of drill holes is unnecessary, but in narrow orebodies, the holes are spaced from 15 to 50 ft. (4.6 to 15 m.) apart. Ten years ago, very few assays were kept of the drilling, but during recent years records have been kept very accurately, showing the location, elevation, assays, and also the vertical section of the hole. After the orebody is reached, cuttings are taken every 2 or 3 ft. (0.6 to 0.9 m.) samples being sometimes taken by pouring the water off the cuttings and taking a portion of the coarse material for assay. It has been found, however, that very often the sludge material poured off with the water contains high mineral values. To overcome this, cuttings from each 2 or 3 ft. are put in a container and after the water is evaporated, sample for assay is taken by means of Jones samplers. Permanent records of cuttings showing various formations are kept in glass jars or glued on large cards. Drilling at present is costing from $1.25 to $1.50 per foot. In pre-war times, the drilling costs ran from 75c to $1 per foot.

Jan 9, 1917

By Carleton Ellis

(Presented at a meeting of the New York Local Section of the Institute, Apr. 12, 1912.) I. INTRODUCTION. THE problem of the influence of hot surfaces upon gaseous combustion is one which, from a purely scientific stand-point, has engaged, for many years past, the attention of Prof. William A. Bone, of Leeds University and the Imperial College, London; and as his recent work has been the direct outcome of earlier scientific investigation, it will be appropriate, by way of introduction, to review briefly the present position of science with respect to this important subject, as stated by Professor Bone. One may perhaps best arrive at an understanding of the term " ?flameless " or " surface " combustion by considering certain facts which differentiate it from the more familiar processes of combustion as they occur in ordinary flames. All hot surfaces have an accelerating influence upon chemical changes in gaseous systems. If, at any temperature, a gaseous system, A, tends to pass over into another system, B, contact with a solid at the same temperature will accelerate the process. To take a very simple example, if a mixture of hydrogen and oxygen in their combining proportions (electrolytic gas) were maintained in an inclosure with smooth glass walls at a temperature of, say, 450° C., there would certainly be a tendency to form steam, but the rate of change would be negligibly small. If, however, there were brought into the system some porous solid material at the same temperature, so that a large surface was exposed to the gases, the rate of change would at once be rapidly accelerated in the layer of gas immediately in contact with the hot surface. Steam, the product, would diffuse outward from the surface, and the supplies of hydrogen and oxygen at the surface would be renewed by diffusion inward. Thus combustion would proceed heterogene-

Sep 1, 1912

By R. I. Jaffee, C. M. Craighead, G. A. Lenning

The a-p type alloys are subject to a loss of tensile ductility with increasing hydrogen content. No hydride phase is visible in embrittled a-B type alloys. The embrittlement encountered appeared to be of the strain-aging type. Both compositional and structural factors are shown to influence the hydrogen tolerance of a-B type alloys. IN previous papers by the authors, the effects of hydrogen on the structure and mechanical properties of high-purity and commercial-purity titanium were described. It was shown that the presence of hydrogen in these materials results in a hydride phase having low solubility at room temperature. This insoluble phase had little effect on the room temperature tensile properties, but did decrease the notch-bar toughness to a large degree. The binary Ti-H systemz indicates that hydrogen is much more soluble in £ than in a-titanium. Hence, it is not expected that the embrittling effects of hydrogen in a-fi alloys will be similar to that found in a alloys. Materials of this type studied in the present investigation included two commercial a-/3 alloys, Ti-8Mn and Ti-4A1-4Mn; three high-purity Ti-Mn alloys containing 3, 6, and 9 pct Mn; and four high-purity Ti-Mo alloys, Ti-SMo, Ti-10.9M0, Ti-13.1 M0, and Ti-20M0, of the a-B and B types. Materials and Fabrication—The high-purity base alloys, composed of iodide titanium and high-purity metals, were prepared by double arc melting under argon in a water-cooled copper crucible, using a water-cooled tungsten electrode. Radiographic examination showed homogeneous Ti-Mo alloys. The analyses of the alloys used in this investigation and their as-fabricated hydrogen content, where determined, are listed in Table I. The two commercial alloys were 1/2 and % in. diam bar stock. No analyses other than hydrogen content were made. In order to maintain the a-B relationship existing in the two commercial alloys, vacuum annealing and hydrogenation were carried out in the B field prior to final fabrication. Fabrication then was done by The three high-purity Ti-Mn alloys were forged to 3/4 in. diam rods at 1600°F, and hot swaged to 1/2 in. diam at 1380°F. Machined and degreased bar stock was vacuum annealed or hydrogenated, fabricated to 1/8 in. diam rod by hot swaging, annealed in argon for 1 hr at 1380°F !75O°C), and water quenched. The six yz lb Ti-Mo ingots were forged to Wi in. diam rods at 1600°F and then hot swaged to % in. diam. Machined and degreased specimens were vacuum annealed or hydrogenated in the /3 field, prior to fabrication, by swaging to Y4 in. rod at 1400°F. After fabrication, the 5 and 10.9 pct Mo alloys were annealed in argon for 16 hr at 1290°F and water quenched to give equiaxed a-B structures. The higher molybdenum content alloys were argon annealed 4 hr at 1470°F and water quenched to give all £ structures.

Jan 1, 1957

By J. H. Faulk

An examination is made of the various factors influencing drilling rate and drill bit life in various diameter holes. It is concluded that drill bits in the size range 4% to 6 1/4 in. can be used to attain substantially the some daily drilling progress as conventional size bits in soft rock drilling operations. An examination of the most important factors influencing "hazard of losing the hole" in the different hole size results in the conclusion that the smaller hole sizes can probably be drilled at reasonably low risk. However, this risk will be somewhat greater in the smaller diameter holes, requiring that special drilling and mud engineering practices be used to make small diameter holes practicable in soft rock drilling operations. An engineering analysia is made of the power and hydraulic requirements of several drill string-hole combinations to test the feasibility of drilling .small diameter holes in soft rock areas. Large econormies in rig power requirements appear possible by drilling .smaller .size holes in these operations. INTRODUCTION The industry now is re-examining the utility of small diameter holes in the light of substantial technical advances made in recent years. Faced with increasing cost of finding reserves and with proration after developing them, the industry must either develop methods of economizing or receive a lower rate of return on investments. Small diameter holes appear to involve an attractive method of economizing. Our objective is to determine if this is technically possible in soft rock operations. Soft rock, as used in this report, refers to those formations of a "drill-ability" corresponding to that of all Gulf Coast formations shallower than and frequently including much of the Eocene rock system. An important phase of technology which we shall examine is relative drilling rate and bit footage which may be obtained with various size bits. Rig operating efficiency, particularly as influenced by hazard, is also discussed in detail. The technical conclusions resulting from these examinations are used to develop sample drill string design and rig horsepower requirements for drilling holes as smaH as 4 3/4 in. and larger. The principal criterion used for the drill string design is that approximately the same daily drilling progress would be possible in all size holes in soft rock operations. This facilitates a comparison of rig size required for drilling the hole sizes in the range between 4 3/4 and 8 3/4 in. BROAD PROBLEM OF DRILLING RATE AND BIT FOOTAGE The three factors controlling daily drilling progress are: (1) drilling rate of bit while on bottom turning, (2) bit footage, and (3) rig operating efficiency. Let us look now at the first two of these factors. Drilling technology has progressed to the point that a semi-quantitative analysis of the effect of various operating variables upon these factors can be made. Those factors which apparently limit both drilling rate and bit footage for bits now in use are: (1) bit design, (2) weight on bit, (3) hydraulic cleaning capacity for bit cutting surfaces and hole bottom, and (4) rotary speed. (We neglect the effect of mud and formation properties because these factors arc the same for the various size bits.

Jan 1, 1957

By O. D. Gonzalez

ThIS communication presents the results of a determination of the permeabilities of hydrogen and deuterium in a iron from 360° to 560°C. Recently Heu-mann and primas' have given values of the diffusivity and solubility in a iron of the two isotopes from which the permeability can be calculated. The work reported in the present communication, however, is a direct measurement of the rate of permeation of the isotopes through an identical iron specimen under the same conditions, so that systematic errors can be minimized in the calculation of the ratio of the permeabilities—the value which is usually of main importance in establishing limits for isotopic differences in diffusive processes. Experimentally the procedure used was the usual one: a steady-state flow of gas produced by a pressure difference across an iron membrane was observed as the pressure rise with time in a previously evacuated, calibrated volume connected to the outlet side of the membrane, while a constant pressure of gas was maintained on the opposite inlet side. The membrane was a cylindrical tube 9.38 cm long, 0.730 cm inside diam, 0.187 cm wall thickness, fabricated of 99.95 pct vacuum-melted National Research Corp. iron (less than 0.003 pct C). One end was sealed by a heliarc-welded iron (99.95 pctj lid of 0.147 cm thickness; the other end of the tube was welded to a 304 stainless-steel tube (0.318 cm ID and 0.318 cm wall) which connects to a vacuum system and to the calibrated volume including a dibutylphthalate manometer. The temperature of the iron membrane was maintained constant to ±0.l°C and was measured with an iron-constantan thermocouple which was calibrated against a standard Pt/Pt-Rh thermocouple: the temperature variation along the length of the membrane did not exceed ±0.5°C. Hydrogen was allowed to pass through the membrane assembly for 72 hr at 615°C before permeability measurements were begun. The system was tested at temperature before and after the experiments by a substitution of helium for hydrogen in the inlet side; under these conditions the pressure rise observed in the outlet side was negligible at all times. The gases used for the permeability measurements were 99.95 pct Matheson prepurified H2 and 99.7 pct D2 (0.3 pct HD) from the Isomet Corp. The gases were dried with liquid N2 before use. In Fig. 1 the logarithms of observed flows, jt, for a pressure difference of 73.4 cm Hg are plotted against T-1 Each point in Fig. 1 represents the slope determined by a least-square evaluation of a plot of the pressure in the outlet side of the membrane against time, including at least two separate sets of observations. Each point in the figure has an uncertainty of ±0.6 pct arising from the experimental uncertainty in the pressure and time measurements. The standard deviation of the observed pressures from the straight lines in all cases is less than the experimental precision of the measurements. The observed flow, jt, includes a small but not negligible flow through the stainless-steel connection.

Jan 1, 1968

By A. M. Gaudin, C. S. Chang

IN general, fatty acids or their alkali salts do not cause clean quartz to float. However, the presence of multivalent ions, such as the alkaline-earth metal ions and heavy-metal ions, can activate quartz and thus make it respond to soap flotation. The mechanism of activation and soap flotation of quartz has been studied.1-4 The problem was attacked by making flotation tests rather than by careful adsorption measurements on suspensions of ground quartz in solutions containing the activator and the collector. Attempts have been made to determine the adsorption of barium ion and calcium ion on quartz. The results have only qualitative value as the analytical methods were not adequately precise. Artificial radioactivity and progress in radioactivity detection have introduced a new analytical tool, which can have a sensitivity several orders of magnitude greater than that of other methods.5-6 In the experimental work described in this paper the radioactive tracers, barium 140 and carbon 14, were employed. Lauric acid was synthesized, having a radioactive carbon atom and was used with Ba140 to study the adsorption of barium and laurate ions from aqueous solution on ground quartz. Flotation tests, using the vacuum flotation technique,4 were run in conjunction with the adsorption experiments. The object of this investigation was to understand better the reaction mechanism of barium activation and soap flotation of quartz. Methods and Materials Quartz Sample Preparation: Lumps of hand picked quartz, washed free of stains, were reduced in size to -20 mesh in laboratory crushers. The product was boiled in concentrated hydrochloric acid to remove the abraded iron. The cleaned product then was ground dry in a laboratory porcelain mill, using siliceous pebbles, to pass through a 200 mesh screen. The ground product was deslimed by sedimentation at 37 microns. This -200 mesh +400 mesh material was subjected again to boiling with concentrated hydrochloric acid, followed by washing with distilled water and further desliming. The cycle was repeated until no trace of iron could be detected in the wash liquor. During the final washing, the pH of the wash water was checked to insure the complete removal of the acid from the mineral. The quartz then' was rinsed with conductivity water. The resulting product was dried in a drying oven and stored in mason jars. The impurities (spectrographic) were as follows: Al, 0.01 to 0.001 pct; Li, Mg, Mn,, Na, each less than 0.001 pct; Fe and Cu not detected. The specific surface of the quartz sample was determined by the krypton gas adsorption method.7 The average of two measurements was 881 sq cm per g. The calculated specific surface for 37/74 micron quartz particles, using a surface factor of 1.96,8 is 900 sq cm per g. This is in good agreement with the measured value of 881 sq cm per g. Beta-Counting Method: The radioactive isotope of barium used in the experimental work was barium 140. It has a sufficiently long half-life, 12.8 days, emits high-energy beta particles (up to 1.0

Jan 1, 1952

By Niels Hansen

The substructure formed by drawing at room temperature in aluminum (99.5 and 99.998 pct purity) and in recrystallized aluminum aluminum-oxide products containing from 0.2 to 4.7 wt pct of aluminum -oxide was examined by transmission electron microscopy, and the flow stress of the drawn materials was measured by tensile testing at room temperature. A sub-grain structure was present after a reduction in area by drawing of 10 to 20 pct, and the subgrain size was observed to decrease with increasing deformation. The tensile data show that the increase in flow stress (0.2 pct offset) by drawing from 10 to 95 pct depends on the reduction in area, not on the composition of the materials. Dispersion strengthening and subgrain bowzdary strengtlzening contribute to the flow stress, and these strengthening processes have been found to be linearly additive. The flow stress (0) can be related to the subgrain size &) by the Petclz relation = uo + k . t, where go is dependent on the composition of the products and k is approximately the same far all materials. THE microstructure of dispersion-strengthened aluminum aluminum-oxide products consists of small oxide plates distributed in an aluminum matrix. The matrix structure depends on the manufacturing history, and in hot-worked as well as cold-worked products the matrix is divided by subgrain (or dislocation) boundaries. For hot-extruded products it has been shown1 that dispersion strengthening and subgrain boundary strengthening are linearly additive, and the flow stress (0.2 pct offset.) at room temperature has been related to the subgrain size (ts) by a Petch equation,2,3 s = so + k . ts-1/2, where s0, increases with increasing oxide content. For cold-worked products containing subgrains no systematic work has been reported, and it was the aim of the present study to examine the microstructure and the relationship between the flow stress and the subgrain size for such products. The behavior of' aluminum aluminum-oxide products depends on the purity of the aluminum matrix, and aluminum of the matrix purity (99.5 pct) was included in the investigation. The literature contains few data about the behavior of this impure aluminum, and aluminum of a higher purity (99.998 pct) was therefore also examined. As regards the relationship between the flow stress and the subgrain size in cold-worked dispersion-strengthened products, no systematic work has been reported. For aged cold-worked structures containing fine precipitates (Fe-Mo carbide) a Petch relation has been found,4 and it has been shown that the k value NlELS HANSEN is Head, Metallurgy Department, Danish Atomic Energy Commission, Research Establishment Riso, Denmark. Manuscriot submitted January 9, 1969. IMD is approximately the same as in iron, whereas the s0 value is higher owing to the presence of the precipi-tates. Investigations of metals such as tungsten,' ferrous metals,4,6 and molybdenum7 cold drawn or swaged at room temperature have shown that the flow stress can be related to the subgrain size by a Petch relation when ts is taken as the subgrain size perpendicular to the direction of deformation. For aluminum no work has been reported on the relationship between the flow stress and the subgrain size after deformation at room temperature, whereas for aluminum tensile strained at different temperatures in the range -183" to 375°C a Petch relation has been found by taking ts equal to the subgrain size.' In the present study two aluminum materials (99.998 and 99.5 pct) and three aluminum aluminum-oxide products (containing 0.2, 1.0, and 4.7 wt pct oxide) were drawn at room temperature to reductions in area from about 10 to about 95 pct. The structures were studied by transmission electron microscopy, and the flow stress (0.2 pct offset) was measured at room temperature. EXPERIMENTAL Materials. The materials are given in Table I together with the chemical analysis. The three aluminum aluminum-oxide products were manufactured from aluminum powder that had been compacted and Table I. Chemical Analysis of Materials Al203 Fe SI Material wt pct wt pct wt pct 99.998 pct* - 0.0004 0.0012 Aluminum 99.5 pctt - 0.36 0.16 Aluminum AlMD13† 0.2 0.16 0.12 Aluminum- -Oxide AlMD105† 1.0 0.26 0.18 Products SAPISML960s† 4.7 0.22 0.19 *Other impurities: O.0004 pct max each of Cu and Zn (supplier's analysis). †Other impurities: 0.03 pct max Cu. 0.02 pct max each of Mn, Mg, Zn, Ti. Table 11. Mean Diameter of Aluminum-Oxide Particles in Extruded and in Cold--Drawn Aluminum Aluminum-Oxide Products Mean Diam. of A1203-Plates* Material State A AlMD105 Extruded 540 Cold Drawn 97 pct 510 SAP ISML 960 Extruded 770 Cold Drawn 95 pct 820 *The standard deviation of the mean is approx. 5 ±pct.

Jan 1, 1970

By Strathmore R. B. Cooke, Marcus Digre

That calcium will activate quartz for flotation with anionic collectors such as soaps has been known for a number of years,12'3 and the method has been applied to the concentration of various iron ores4 5 6 as well as to other materials. Clemmer gives the permissible pH range for the activation of quartz by calcium as between 9.5 and 12.5 with an optimum value of 11.0, and Hertzog7 has determined the calcium abstraction of iron ores and of Ottawa sand, but otherwise little quantitative data are available. The purpose of the present investigation was to determine those conditions under which dilute solutions of calcium chloride will activate quartz for anionic flotation and to determine the amount of calcium ion adsorbed by quartz. Those variables, the influence of which was primary, such as calcium, sodium, and hydrogen ion concentrations, were studied. Other factors which influenced the results are discussed in the description of the experiments. Three different experimental methods were used to determine the activation of the quartz. The first method was to treat a sample of ground, deslimed quartz with solutions of calcium chloride and sodium hydroxide, and to determine the calcium adsorbed by chemical analysis of the solution. Advantages are that a direct value for the amount of calcium adsorbed is obtained, and introduction of a collector which may affect the adsorption is avoided. The difficulty is to determine the extremely small differences in the calcium concentrations before and after the abstraction. The second method was to determine the activation of the quartz by observing the contact angle obtained on pressing an air bubble against the polished surface of a piece of quartz immersed in a solution of calcium chloride, sodium hydroxide, and sodium oleate. This is the well-known "contact angle" method. The third method was to determine those conditions under which an air bubble will pick up quartz particles immersed in a solution of the desired reagents. Disadvantages common to the sec- ond and third methods are that introduction of a collector is necessary to obtain bubble contact with the mineral; very small quantities of contaminant can give erroneous results; and no information is obtainable concerning the amount of calcium adsorbed. Advantages are that tedious analyses, which at best give approximate results, are avoided, and the conditions, especially for the third method, closely simulate those of actual flotation. Although the most consistent results were obtained with the third method, this paper describes the techniques used and the results obtained from each of the three methods. Distilled water and analytical grade reagents were used throughout except where otherwise stated. Between tests all glass articles were cleaned with a chromic-sulphuric acid mixture and sodium hydroxide. Abstraction Method The raw material for the tests was Ottawa sand sized between 14 and 28 mesh. Batches of 500 g of this sand were dry ground for 1 hr in an Abbe porcelain mill with 2700 g of quartz pebbles. The batches were split down to samples weighing approximately 30 g, and the weight of each sample was adjusted to exactly this value.

Jan 1, 1950

By Thomas P. Forbath

THE sudden realization that known sulphur reserves amenable to mining by the Frasch hot water process are nearing exhaustion focused attention on widely scattered surface deposits throughout the world. These deposits are not necessarily of lower sulphur content than ores located underneath Louisiana or Texas salt domes which usually average about 30 pct sulphur disseminated in limestone matrix. Their near surface occurrence, however, renders exploitation by the Frasch process impossible. As is well known, the Frasch process depends on the presence of 500 to 1000 ft of overburden and cap rock above the sulphur deposits to permit melting underground sulphur in place by diffusing hot water under pressures of 200 to 600 psig in the formation and raising the molten sulphur to surface by air lift. This process renders possible the production of pure sulphur which is 99.5 pct pure without any subsequent treatment. Surface deposits contain sulphur in the same range of concentrations as the salt dome deposits, i.e., from 10 to 50 pct sulphur, associated with various gangue materials such as silica, limestone, and gypsum. The pirincipal distinction, then, does not lie in the percentage of sulphur contained in the ore, but in the geological nature of the deposit. A recent study' of the world sulphur supply situation estimated 1950 sulphur production in the free world countries at 5.6 million long tons, of which the United States produced 5.2 million tons, or 93 pct of the total. While America's domestic needs alone would have been covered by national production, about 1.4 million tons were exported during the same year. Despite all the steps which are being taken to restrict use of elemental sulphur and to force the fullest possible development of alternate sulphur sources here and abroad, the deficit in elemental sulphur production will probably increase with time. As a result of intensive prospecting for oil throughout the Gulf Coast area discovery of significant new salt domes is held unlikely. With the growing scarcity of sulphur and what appears to be an inevitable rise in price, recovery from deposits not amenable to Frasch-process mining assumes greater economic importance. Untapped Reserves The most important deposits in this category are located in Sicily, where elemental sulphur occurs in Miocene limestone and gypsum formation. Sulphur content of these ores ranges from 12 to 50 pct with an estimated average of 26 pct. Although quantitative estimate of these reserves is not available it is held that they exceed 50 million tons of sulphur. Similar deposits occur also on the mainland which contribute about one-third of Italy's total current annual production of 230,000 tons, but these are known to be nearing exhaustion. Significant surface deposits of volcanic origin are located in South America, Japan and western United States, silica being characteristic gangue con-stituent. The largest of these deposits are in South America. More than 100 extend over a zone 3000 miles long, paralleling the west coast of South America. 'Total sulphur content of these deposits has been estimated to be as high as 100 million tons. The main islands of Japan also possess at least 40 known volcanic sulphur deposits with probable reserves of 25 to 50 million tons.' Prospected reserves in western United States might amount to 2 million long tons, principal deposits being located in the northwestern part of Wyoming, southern Utah, and eastern California. Volcanic deposits of lesser importance are found around the Mediterranean, in Turkey and Greece, and in Africa, Egypt, Abyssinia, and Somaliland. Beneficiation Methods Different methods of beneficiation have been used in these various locations. In Italy the Calcarone kiln and Gill regenerative furnaces are used exclusively. Both utilize heat liberated by burning part of the sulphur in the ore to liquify or vaporize the remaining sulphur, which is recovered by solidification or condensation. The Calcarone kiln is of conical shape, generally 35 ft in diam at base and 18 ft high. A kiln of 25,000 cu ft capacity burns for about two months and yields about 200 tons of sulphur. The Gill furnace consists of a series of chambers with domed roofs. Sulphur is burned and melted in one chamber at a time and the hot combustion gases are used to preheat the ore charge in the subsequent cell. These furnaces operate on a cycle of 4 to 8 days. The recovery yield of both systems is about 65 pct. Sulphur losses amount to 25 pct through the combustion to sulphur dioxide; about 10 pct is retained in discarded calcines. Ores containing less than 20 pct are not considered suitable as furnace feed. These methods are not only wasteful because of the low recovery obtained, but represent a serious atmospheric pollution problem. Sulphur produced ranges from 96 to 99 pct purity and thus does not match Texas or Louisiana sulphur. Owing to the present shortage, sulphur in the Middle East sells

Jan 1, 1954

Lester Guttman (General Electric Research Lab-boratory)—Seybolt has measured the thermodynamic activity of silicon in dilute solution in a iron. The anomaly which appears at 800 °C in the approximate range 1 to 6 wt pct Si is most naturally attributed, as Seybolt has done, to the existence of a region of

Jan 1, 1960

By H. E. Cook

The Ising model for the internal energy of a binary alloy has been used to obtain a general equation for the critical resolved shear stress of partially ordered crystals. The equation expresses the stress in terms of the Warren "alphas " and can be used to estimate the variation in strength with order without the assumption, present in the original formulation of this problem in terms of domain size, that order is complete within each domain and that the domains are of ungorm size and shape. In addition, it is the general equation, according to the Ising model, for strengthening by short-range order. Two applications of the equation are considered: One is an estimate of the variation in strength of CkAu with long-range order. The other is an estimate of the variation in strength of FeCo with quench temperature. Reasonable agreement is found with the variations reported in the literature. When the internal energy of an alloy crystal depends upon the distribution of solute, the strength of the crystal will also depend upon it because a portion of the applied stress for plastic deformation will be: where V is the volume of the crystal and E(E) is the energy change associated with the solute redistribution caused by the plastic strain, E. We expect T to equal zero for a crystal having a random arrangement of solute because the arrangement would remain random after plastic deformation. Likewise, we expect it to equal zero when the crystal is perfectly ordered because the motion of paired dislocations found in such crystals does not disrupt order. However, when short-range order exists or when long-range order is incomplete, plastic deformation will decrease the amount of order and additional work, proportional to the ordering energy, will be expended. Fisher' estimated T for crystals having short-range order by assuming an interaction energy between neighboring atoms and estimating the change in the number of unlike neighbors as a dislocation moved through the crystal. (His analysis was limited and several workers2"6 have since given more complete ones.) Fisher minimized the importance of a strengthening mechanism of this type for paired dislocations in a structure having long-range order. ~ottrell,' however, pointed out that T could be appreciable for ordered crystals having antiphase domains. He attributed the strengthening to the increase in surface energy of the domains as they were cut by paired dislocations. Ardley,' in his test of Cottrell's theory, found that r for Cu3Au crystals obeyed the equation: for 1 > t where 1 is the domain size, t is the domain wall thickness, and y is the surface energy of an antiphase boundary. His experiments represent the classic confirmation of the strengthening mechanism proposed by Cottrell. However, the assumptions involved in using Cottrell's theory are valid only for large domain size in CU~AU,~"~ i.e., when Eq. [2] reduces to: For small domains, ~linn~ has questioned Ardley's assumption that order was complete, and, indeed, Stoloff and ~avies" fpnd it incomplete until a size of approximately lOOA was reached. Even when the order within a domain is complete, it is not obvious how one determines the appropriate value for I in a structure where domains vary in size and are irregularly shaped. The purpose of this paper is to estimate T without restrictions upon the degree of order and domain shape. Our major assumption will be the use of a generalization of the model proposed by Bethe" (the Ising model) for the internal energy. This will in fact allow us to combine the theories for strengthening by short-range order and by antiphase domains into a single, general formalism. We will use the results to estimate the variation in strength of Cu3Au crystals with long-range order8 and the variation in flow stress of FeCo crystals with quench temperature.12'13 INTERNAL ENERGY For simplicity, we restrict our considerations to those binary solid solutions which can be described as an arrangement of atoms on a Bravais lattice. An atom site will be indexed by three numbers (PI, pz, p3) determined by the vector: from the origin fixed at atom (0, 0, 0) to the atom site where a', an, and a, are the lattice translation vectors. We write: For the energy of the crystal where pi(p) is the probability (either zero or one) of finding an atom of type i (i = 1, 2) at site (p), which is shorthand for (pl, pz, p3) and pj(p + r) is that for an atom of type j (j = 1, 2) at the site (p + r), which is shorthand for (pl + rl, The coupling parameter, resents the energy associated with the pair Pi(p), Pj(p + r). The crystal is assumed large enough so that surface effects can be neglected; therefore, trans-lational and inversion symmetry require the coupling parameters to obey the relations

Jan 1, 1969