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By J. E. Hilliard, J. W. Cahn

calculation has been made of the standard deviations to be expected in the measurement of volume fractions by areal analysis, lineal analysis and four point-counting Procedures. The effect of experimetztal errors is not included. Our conclusion is that a point count using a two-dimensional grid will be the most efficient method of volume fraction analvsis providing the grid spacing IS coarse enough. The predicted standard deviation for such an analysis is shown to he in good agreement with that determined experimentally. A metallurgist wishing to estimate a structural property by means of quantitative metallography is often faced with a choice between several different procedures. In such a case, he will naturally wish to know: a) Which procedure is the most efficient in the sense of requiring the least effort for a given precision? b) For a given procedure, what are the conditions for maximum efficiency? c) Under these conditions, how many measurements are required to attain a given precision? It is our aim in this paper to provide at least partial answers to these queries as they relate to the estimation of volume fractions from measurements on a random two-dimensional section of an opaque specimen. The commonly used techniques1,2 for volume-fraction analyses are based on one or more of the following principles: i) For an areal or Delesse3 analysis: That the areal fraction of a three-dimensional feature intercepted by a random plane provides an unbiased estimate of the volume fraction of that feature. ii) For a lineal or Rosiwal4 analysis: That the fractional intercept on a line passing at random through a two-or three-dimensional feature provides an unbiased estimate of, respectively, the areal or volume fraction of that feature. iii) For a point-count analysis: That the fractional number of randomly or regularly dispersed points falling within the boundaries of a two-dimensional feature on a plane, or within the boundaries of a three-dimensional feature in a volume, provides an unbiased estimate of, respectively, the areal or volume fraction of that feature. The absence of bias referred to in these principles does not, of course, imply that the results of an analysis will be free of error, but only that the expected result is equal to the true one. Application of the foregoing principles provide the following six possible experimental procedures: a) An Areal Analysis—This involves the measurement with a planimeter (or other means) of the area of a constitutent intercepted by the plane of polish b) A Two-Dimensional Random Point Count—Apos-sible experimental procedure for this analysis is to superimpose a sheet of transparent graph paper on a micrograph, and then use a table of random numbers to select coordinates for the points. c) A Two-Dimensiotuzl Systematic Point Count-Similar to b) except that the points are distributed in a prescribed manner, usually at the corners of a lattice superimposed on a micrograph or the screen of a projection microscope. d)A Lineal Analysis—A measurement of the fractional line length intercepted. It is usually performed by traversing the specimen under the cross hairs of a microscope and recording the distance travelled in each constituent. e) 4 One-Dimensional Random-Point Count— This could be performed by traversing the specimen with stops at random intervals to identify the constituent then present under the cross hairs. f) A One-Dimensionul Systematic Point Count— Similar to e) except that the traverse is stopped at prescribed (usually equal) intervals. It will be noted that the point-counting procedures b) and c) can be regarded as methods of estimating the areal fraction. Similarly, e) and f) are indirect methods of making a lineal analysis. All of the six procedures described above involve at least one stage of sampling. Thus, quite apart from any experimental errors, there will always be a statistical uncertainty associated with the final results. It is with the calculation of this uncertainty that we will be concerned. To avoid unnecessary repetition, the statistical relationships that will be used in the calculations are collected together in the appendix. For a fuller discussion reference should be made to one of the many textbooks5,6 on statistics. For symbols relating to the specimen structure we will follow as far as possible the terminology used by Smith and Guttman.7

Jan 1, 1962

By E. V. Crane

A tremendous volume of the metal rolled annually into sheets strips and coil stock finds its way to a host of stamping and manufacturing plants which are the quantity production units of the country. Considerable in volume, too, are the rolled and extruded rods which go into forging and manufacturing plants for conversion into the same general line: those widely sold metallic necessities and luxuries of the household, the office, transportation, farming and building construction. Yet, in spite of its age and its importance, the stamping trade has been doing its "engineering" largely by trial and error. Its distinctive method is shearing out and plastically working metal to finished shape in a few quick strokes with high loads and expensive tools which are warranted only by large quantities to be produced. The principal operations have many features In common with rolling and wire-drawing methods. Combinations of stresses are diffcrent, however, and details of operations are infinite in variety. An engineering study of the subject begins with stress analysis, but must go back to metallurgy for its foundation. A grouping of pressed-metal working operations according to whether the metal is (1) sheared, (2) bent, (3) drawn or (4) squeezed has proved useful. All of these groups include instances of both hot and cold operations. For discussions of metal working properties, the division between hot and cold working is taken as the recrystallization range of temperature. This, of course, brings tin, lead and often zinc into the hot-work range at or near room temperature. The outstanding hot-working press field is in forging: particularly of brass; all of which is included in the squeezing group. Shearing Operations The shearing group of operations, including blanking, piercing, trimming, shaving, slitting, shearing, notching, parting and numerous variations and combinations of these enters once or more into the production schedule of practically every stamped or forged article. The transverse stress, set up in shearing, as shown in Fig. 1A, is a combination of an angular compressive thrust and a tensile stress which is also at an

Jan 1, 1931

By Harrison Schmitt

SINCE the U. S. Geological Survey published the data on the Central Mining District collected by Lindgren and Graton1 and by Paige2 much new information has been obtained by development and mapping, but none of it had been published until recently when Kniffin3 published on Fierro, Lasky4 on the Ground Hog mine, Thorne5 on Santa Rita and Landon6 filed a thesis on the Fierro-Hanover-Santa Rita area at the Uni-versity of Chicago. During the years 1927-1930 much of the writer's time was spent in mapping the geology and ore deposits of this district, particularly in the area of the zinc deposits at Hanover. Some of the data collected are presented here. Previous publications have been freely drawn upon and additional data used that were generously supplied by L. M. Kniffin, Wilfred Wright and Gerald Ballmer. Thanks are due Augustus Locke, Samuel G. Lasky, Kniffin, Wright and Ballmer for suggestions and critical readings of the manuscript, and to the Empire Zinc Co. (a subsidiary of the New Jersey Zinc Co.) for the privilege of publishing material compiled largely at its expense. The relation of the Central. or the Santa Rita-Hanover-Fierro district to the Silver City district is shown on Paige's geologic map in the Silver City folio.7 Granodiorite porphyry and quartz-monzonite porphyry

Jan 1, 1933

Report of the Secretary TO THE BOARD OF DIRECTORS OF THE AMERICAN INSTITUTE OF MINING AND METALLURGICAL ENGINEERS Gentlemen:-To a Board of Directors keeping in as close touch with all of the affairs under their care as do the Board of Directors of the A. I. M. E., through their monthly meetings, a report of the year's progress is almost superfluous. To the members who read the monthly reports of. the Board Meetings and of the various activities of the Institute as published each month, a yearly report cannot carry much fresh information; yet for both it may be well, as is the custom, to glance over the field of our activities during the past year, and to make an estimate for the year to come. The beginning of 1924 was not propitious for the members of the mining profession, though tonnage production for 1923 had been high and the gross value higher than for several years. The margin of profit had been narrow, prospecting and development were limited, and many of our members were unemployed, or were working in other industries. Toward the end of the year, higher metal, prices were in sight. Old-time optimism began to grow, and it now brightens the outlook for 1925. An excellent barometer of the prosperity of the industry, and that of the Institute, for they go hand in hand, is the work of our Employment Bureau. During the past few months, the percentage of our members for whom openings have been found has been increasing to a marked extent, and many members who had fallen in arrears are placing themselves in good standing. The number of new members joining has remained about as it was in 1922 and 1923. The Directors have reason to congratulate themselves on the interest maintained during a dull period, for it is not humanly possible to take a keen interest in the technology of an industry when our hands and minds are not actively engaged in it Now, with a much brighter outlook, we can look forward to a year of increasing prosperity for the industry and for the Institute.

Jan 3, 1925

By H. M. Howe

It has seemed to the writer that one important, and indeed sufficient reason, for our slow progress in learning the relation between the chemical composition and the physical properties of cast-iron, has been that the problem has not been attacked properly. It would be well to select the most probable working hypothesis which we can find, and proceed to test that hypothesis by comparison with observed facts, and by making new observations specially designed for such a test. Our first step, then, is to select the most probable working hypothesis ; and to attempt this selection, to state the hypothesis and its immediate corollaries, and to take some first steps toward testing it, is the object of the present paper. Its chief purpose is to bring the hypothesis to the attention of those who are more familiar with the evidence than the writer can pretend to be, and in a better position both to present new evidence and to discuss it. The hypothesis here selected is, that composition governs properties in the case of cast-iron, in the same general way and for the same reasons as in the case of steel, mutatis mutandis. This hypothesis, which of course makes no claim to originality, certainly seems reasonable and probable; its exposition and discussion are made easy by our existing knowledge of the constitution of normal or " carbon " steel; it therefore seems worthy of consideration.

Jan 1, 1902

By Leroy A. Palmer

All the domestic production of magnesite during 1925 came from two states, California and Washington. Of a total of 120,660 tons of crude ore, 64,600 tons, or 54 per cent., were produced in California.' Of this quantity California produced about 99 per cent. of the caustic calcined, but only 10 per cent. of the dead-burned. The largest producer was C. S. Maltby, of San Francisco, who operated the Red Mountain mine, in Santa Clara County, and the Sampson mine, in San Benito County, under lease. These two mines have been studied by the author, and offer interesting comparisons as to mining and treatment methods and final products. Geology The general geology of the magnesite deposits of California has been described by Hess,2 Bain3 and others4 and although a detailed discussion is not necessary here, a brief summary will assist in understanding mining conditions. California magnesite, when comparatively pure, is usually a white, fine-grained rock, with a conchoidal fracture, occurring in veins and lense-like masses in serpentine. The veins vary considerably in width, and usually occur in a series of more or less parallel veins intersected by other series or systems of veins, probably following original or secondary fissures in the enclosing serpentine. The most generally accepted theory of origin is that the magnesite was formed by the action of surface waters charged with CO2 percolating downward through fissures and changing the magnesium silicates of the serpentine into magnesium carbonate.

Jan 1, 1927

By Julius Pohlman

The history of Niagara Falls, as currently told, is simple, and by that very simplicity it has been rendered plausible. AS the story runs, the Falls were once situated at Lewiston, 7 miles to the north of their present site; and, since all the rocks in this section are alternate hard and soft strata, the waters acting readily upon the soft shales caused their removal, and the overlying hard lagers, deprived of support, broke down under the weight of the large volume of water that rushed over them; and this erosive action has sent the edge of the fall more and more southward, until it now has excavated the seven-mile gorge between Lewiston and the village of Niagara Falls. (See Fig. 1.) As early as 1790" we find this theory advanced in a description of this region; and it has been practically endorsed by subsequent observers, the most prominent of whom was Prof. James Hall, the State Geologist of New York, who surveyed the Falls in 1841, and gave the most exact description of their surroundings in the publications of the State Survey.? Not until 1883 was the correctness of the accepted theory of the Falls questioned.‡ The geology of the basins of the Great. Lakes, as elucidated by Newberry,§ Speneer,ll and others, has added largely to a clearer understanding of the life-history of the Falls. The investigators have shown us that Lake Erie, as a lake, is, geologically speaking, quite young; that its valley was excavated in pre-glacial times by a series of rivers; and that the Maumee, Sandusky, Cuyaboga, Alleghany and other rivers carried the drainage of the surrounding

Jan 1, 1889

By A. T. Tye

REGARDING the results of preferential flotation at Cananea, Weinig has stated that "The concentrating mill of the Cananea Consolidated Copper Company at Cananea, Mexico, furnishes an excellent example of modern flotation practice. The complete figures are given because they present so forcibly the advantages of modern selective flotation."' L. 0. Howard notes that "Perhaps the outstanding example so far published of improvements in results through the use of selective flotation is that at Cananea, Mexico."2 The following notes indicate the conditions under which the results were obtained at Cananea; also the effect of preferential flotation at the concentrator and at the smelter. In the majority of cases the full benefit of selective flotation is not fully realized, as the concentrates are shipped from the mill to smelters owned by other companies. The saving made at a certain concentrator by this method of flotation may be well understood but the saving resulting at the smelter from the results of preferential flotation at the mill is not so apparent, as the data are contained in the smelting records of some other company. Even at the smelter the great gains following preferential flotation may not be noted, as a variety of ores and concentrates from various sources are received and the difference from the changed concentrator operations of a certain mill may be obscured. As noted by Professor Weinig and Professor Howard, the results obtained at Cananea brought about a veritable metallurgical revolution at the smelter.

Jan 1, 1927

By John A. Church

IT is a well-known fact that under similar conditions a ton of pig iron can be made from any ore with less fuel when charcoal is used than when coke or anthracite is employed for heating. The cause of this superiority is entirely undiscovered, and no explanation has yet been offered which has won even temporary acceptance. Such as they are the hypotheses heretofore presented are of two general kinds, and they come from those two divisions of the working force which are so often antagonistic in all professions, the scientific and the practical men. The theory of the scientific men is drawn from the chemical reactions which are known to go on in the furnace, and it is well expressed in a recent paper by Prof. Akerman, of the Stockholm (Sweden) School of Mines. It makes the superiority of charcoal as a fuel in the blast furnace to depend upon its quick and thorough reduction of carbonic acid. This property belongs to charcoal in virtue of its porous structure. Its cells have a diameter of only one twenty-four hundredth of an inch, and one grain of charcoal has been computed to have a surface of two and four-tenths square feet. According to the theory in question, carbonic acid is formed by the first impact of the air upon the fuel; but in charcoal furnaces the acid is immediately reduced to oxide by taking the necessary amount of carbon into combination, and the gas reaches its highest reducing power even in the near vicinity of the tuyeres. Coke, being harder, does not produce so strong a reducing gas in that part of. the furnace. Carbonic acid is formed as in the case of charcoal, and remains longer before its reduction to oxide is completed. Anthracite is the

Jan 1, 1879

NORTH AMERICA Number Members Alaska 36 Canada 323 Mexico 184 Newfoundland 3 United States Alabama 40 Arizona 111 Arkansas 8 California 646 Colorado 171 Connecticut 90 Delaware 21 District of Columbia 136 Florida 16 Georgia 7 Idaho 66 Illinois 208 Indiana 66 Iowa 11 Kansas 24 Kentucky 32

Jan 1, 1934

By Ove Sandberg, Olav Bowitz

The operational characteristics of the Soderberg vertical spike anode are briefly discussed stressing the importance of the flow properties of paste in the fluid zone, the thermal shrinkage in the carbonizing zone, and the surface disintegration in the consumption zone. The requirements for paste recipe and binder quality are combined with design and operation of cell. A low temperature susceptibility of viscosity and low thermal shrinkage of paste together with a low microporosity of the binder coke are important properties. PRACTICAL application of Soderberg's idea of a selfbaking carbon electrode proved successful just before 1920. Shortly after, experimental work was started with the aim of developing a continuous electrode that could be adopted as anode in aluminium reduction cells. The intermittent operation of a large number of small prebaked anodes made the idea of developing a continuous anode for electrolytic production of aluminium especially tempting. Moreover, the electrode consumption in this process, even on a theoretical basis, is very high. Many installations were carried out in the 1930's and during the Second World War. During the tremendous post-war expansion of the aluminium industry, the Soderberg electrode has been steadily more widely adopted. Thus, today more than 60 pct of the Western World's output of aluminium is produced in cells with selfbaking anodes, see Big. 1. The quality of the anode paste of Sfiderberg elec- trodes is considered a major factor influencing the specific carbon consumption. The purpose of this paper is to survey the fundamental requirements which must be met in order to obtain good anode operation. We have limited this paper to a discussion of Elektrokemisk's research on the vertical spike type anode. I) FUNDAMEKI'TALS OF ANODE CARBON PERFORMANCE A) Brief Introduction. The only practical method for producing a conductive carbon anode of the size required is to form and carbonize a mixture of a carbonaceous binder and a precalcined dry aggregate coke. In the Soderberg electrode, the forming and carbonization take place in the electrolytic cell

Jan 1, 1962

By R. F. Shurtz

The author proposes a method used with some success on a magnesite deposit at Gabbs, Nev. He believes this procedure to be more sound than the blind practice of assigning uniform quality to large, soinetimes vast blocks or ore on the basis of analyses made of a small number of samples. When an ore deposit is evaluated on the basis of core sampling, questions always arise as to how much weight should be given the various sample grades and how the deposit should be divided into specific volumes assigned to corresponding grades. For a tabular deposit it is customary to use the so-called zone-of-influence. This zone is usually defined as the polygon in the plane of the deposit having corners halfway between a given core drill intersection and each of the nearest neighboring intersections. The volume of the ore in this polygon is assigned the analysis obtained from the drill core taken at the intersection. In massive or irregular deposits, volumes of various shapes may be defined with respect to the locations of drill core samples. These volumes may be regarded as three-dimensional zones-of-influence; the theory involved in assigning the values of the central analyses to the ore in the volumes is the same as that used in the case of a tabular deposit. The zone-of-influence method was used in evaluating one of the magnesite deposits at Gabbs, Nev.'-"

Jan 1, 1960

By B. C. Craft

The principal events in the oil and gas operations for Louisiana during 1933 have been the rapid development of the Converse field in Sabine Parish, the discovery of three new salt domes, one in North Louisiana and two in South Louisiana, increased development in the Iowa field on the Calcasieu-Jefferson Davis Parish line, and extensive geophysical operations over a wide territory. Other miscellaneous events worthy of mention are the continued leasing of prospective oil lands over a wide area, extension of production at the East Hackberry field, Cameron Parish, discovery of deep sands at Caillou Island, Terrebonne Parish, and the completion of several important wildcats. Despite proration, oil production showed a substantial increase during 1933. The total output for this area was 25,599,802 bbl. as compared with 22,507,387 bbl. during 1932. North Louisiana There were 111 oil wells and 47 gas wells completed in North Louisiana during 1933 as compared with 109 oil wells and 33 gas wells during 1932. North Louisiana oil production decreased approximately 692,625 bbl. in 1933 from its 1932 figure. The normal decline in the old fields was partly offset by increased production at the Zwolle and Converse fields in Sabine Parish. Acid treatment of wells in the Zwolle, Converse and Monroe fields was highly successful. The method of application has been described by H. K. Shearer, Geologist, Pelican Natural Gas Co., as fo1lows:l With tubing in the hole and standing valve removed, the casing is filled with oil to the surface. The limestone solvent is pumped in through the tubing, at the same time bleeding off enough oil from the casinghead to equal the volume contained in the tubing plus the volume of open hole to be treated. The amount of solvent used in most of the wells treated was 1000 gal., which is enough to dissolve about 11 cu. ft. of chalk or limestone. After the computed amount of oil is bled off, the casinghead is closed and the remainder of the solvent is pumped in at whatever pressure is necessary to force it into the oil-producing horizon. The solvent is followed up with enough oil to

Jan 1, 1934

By Will B. Jamison

Man's material advance from one level of civilization to the next has involved the development of new, more useful tools and the utilization of energy greater than he alone could produce. These two essentials for material progress have developed at an ever increasing rate in the last century. While the first really successful use of mechanical energy derived from burning fuel was in James Watt's steam engine which pumped water from coal mines in Cornwall about 1770, there was still very little use of mechanical energy in mining by 1900 except for pumping and hoisting. Compressed air, having some of the characteristics of steam and which operated engines not unlike steam engines or steam hammers, powered the first attempts to mine coal with energy greater than human muscle could provide. When direct current-powered traction cars replaced horse-drawn transportation cars on city streets, it was natural that direct current locomotives should begin to replace animal and human power in mine haulage. Slowly, trolley and battery locomotives were developed and introduced. With d-c systems being established for haulage, it was natural that improved cutting machines should be developed and powered by d-c motors. Thus began the years of

Jan 5, 1960

By N. A. Stockett

SOUTHEAST Missouri is the largest and oldest lead-producing district in the United States. For the year 1941, the statistical picture of pig-lead production, stated in short tons (partly estimated by the Engineering and Mining Journal) is as follows. [Tons World production 2,000,000 United States production 460.000 Southeast Missouri production 242,000] The consumption of primary lead in the United States in 1941 was approximately 900,000 tons, or almost double the country's production. The largest previous year's consumption in the United States was 718,000 tons, in 1926. The largest quantities of lead are used for cable sheathing, storage batteries and white lead. During 1941 tetraethyl lead for auto and aviation gasoline consumed 50,000 tons of lead. The entire lead production of Southeast Missouri is now mined by the St. Joseph Lead Co., whose dominant position as the largest producer in the United States of lead directly from ores is best shown by the fact that in 1941 it produced approximately 31 per cent of the lead production of the United States from its mines in southeast Missouri, where 22,000 tons of ore, averag¬ing over 3.00 per cent lead, is mined per working day. It is known that lead was mined at Mine La Motte, Madison County, Missouri, by Renault in 1723. Other white men and Indians probably did some mining prior to that time. Since 1865, the recorded production to Jan. 1, 1942, shows that the St. Joseph Lead Co. and the various other companies that have operated in St. Francois County mined lead ore, which, after milling and smelting losses produced 5,00,000 short tons of pig lead. About 95 per cent of the present lead production of Southeast Missouri is mined in St. Francois County. The northern part of this area is 60 miles south of St. Louis. The remainder of the lead is obtained at Mine La Motte, about 25 miles southeast from the center of the producing area in St. Francois County. PROSPECTING In this district, most of the ore is discovered by surface and underground diamond drills and by prospect drilling underground with rock drills. Each 2-ft. length of the cuttings from these Jackhamer prospect holes is assayed for lead. These holes are marked and the records are entered on maps. It has been found that close drilling--100-ft. centers of holes, and sometimes less-is necessary in order to locate most of the smaller commercial ore bodies, many of which previously had been missed by drilling the areas with holes spaced 200-ft. centers or more.

Jan 1, 1943

By C. R. Ramachandra, C. C. Patel

Flotation of chalcopyrite from a low grade ore was studied by using different xanthates and dixanthogens as collectors and by conditioning the flotation pulp with oxidizing gaseous systems. The improvement in the recovery of chalcopyrite with the oxidizing systems was mainly due to the auto-activation of chalcopyrite, leading to the enhanced adsorption of xanthates and dixanthogens even when the latter were formed by oxidation of the xanthates. With air or oxygen as oxidizing system, the amount of ethyl xanthate required at pH 8.5 was much less than normally employed in the industry, the recovery being 97-99% of chalcopyrite with a concentrate of 24% copper. With isopropyl and isoamyl xanthates, the recovery was improved but the grade was lowered. By conditioning the pulp with air-CO2 or oxygen-CO2 mixture, the recovery was lowered with ethyl xanthate only, mainly due to the depressant action of bicarbonate formed. Flotation with dixanthogens gave cleaner concentrates of chalcopyrite. because iron pyrite did not float with these collectors. Of the dixanthogens tried, diisopropyl dixanthogen gave the highest recovery, 99% chalcopyrite with a concentrate containing 28.5 to 30% copper, when the pulp at pH 8.5 was condi-tioned with air. Isopropyl dixanthogen was found to be the best collector of all the xanthates and dixanthogens studied. It was found that the adsorbed ethyl, isopropyl and isoamyl xanthates at chalcopyrite surface, activated by cupric sulfate, and at iron pyrite surface were oxidized to the corresponding dixanthogens to different degrees in presence of air, oxygen, air-carbon dioxide mixture and oxygen-carbon dioxide mixture.' The dixanthogen formed at chalcopyrite surface was, however, firmly adsorbed while that at iron pyrite surface was easily desorbed. Since dixanthogens formed have greater hydrophobicity than the corresponding xanthates, as revealed by contact angles,1,2 the former were expected to improve the flotation results. It was, therefore, thought desirable to find out the effect of air, oxygen, air-carbon dioxide mixture and oxygen-carbon dioxide mixture on the selective flotation of chalcopyrite when individual xanthates were used as collectors. The effect of direct use of dixanthogens as collectors on the selective flotation of chalcopyrite was also investigated. For these studies, low grade chalcopyrite ore, received from the Indian Copper Corp., Ltd. (I.C.C.), Ghatsila, Bihar, was employed. At the milling plant of the I.C.C., chalcopyrite is floated at a pH of 8.5, employing ethyl xanthate as collector. EXPERIMENTAL Materials Employed: XANTHATES - Ethyl, isopropyl and isoamyl xanthates of potassium were prepared in a pure state by the methods described earlier.4 A 0.03% aqueous solution of a xanthate was freshly prepared in air-free distilled water for flotation studies. DIXANTHOGENS - Diethyl, diisopropyl and diisoamyl dixanthogens were prepared by the oxidation of xanthates by iodine and purified by extraction with petroleum ether. A 0.03% alcoholic solution of dixanthogen was used as a collector. FROTHER - A 0.2% solution of pine oil in ethyl alcohol was employed. SODIUM CARBONATE - A 0.4 N solution was used. ORE - The composition of the -100 +200-mesh size (Tyler standard) powdered ore, as determined by standard methods of analysis, was: copper 1.57%, iron 10.29%, sulfur 3.15% and acid insolubles 66.10%. Iron present as chalcopyrite (CuFeS2) was 1.38%, while that present as iron pyrite (FeS,) was 1.37%. Both chalcopyrite and iron pyrite were found to be liberated from the gangue minerals and from each other, as observed under a microscope. Flotation of Chalcopyrite with Xanthates in Presence of Different Gaseous Systems: Fifteen grams of -100 + 200-mesh size ore were shaken well with 100 ml of distilled water. The pH of the pulp was adjusted to 8.5 by the addition of sodium carbonate solution. Then 0.1 ml of xanthate solution (0.005 lb xanthate per ton of the ore) was mixed with the pulp, and the latter together with washings transferred to a

Jan 1, 1963

By F. W. Jessen, James N. Howell

The accumulation of paraffin deposits in tubular goods has been recognized as a major production problem since the inception of the petroleum industry. This problem is not limited to any particular geographical area nor is it limited to a specific type of crude oil.' Generally speaking, "paraffin" deposition pertains to the deposition of any predominately organic material in flow lines, and possibly even at the sand face, which would hamper the production of oil. In some fields, a continuous effort is required to remove deposits of paraffin and in order to accomplish this, many unique methods have been devised. The best solution to this problem, however, is to prevent the formation of such deposits. One method which has been tried in a number of fields is the use of plastic pipe. The purpose of this investigation is to compare the relative effectiveness of several plastic materials to aid in the reduction or prevention of paraffin accumulations in surface flow lines. COMPOSITlON OF PARAFFIN DEPOSITS By definition, paraffin deposits are those materials which are insoluble in crude oil at the prevailing producing conditions of temperature and pressure. Such deposits1 s usually consist of small particles of petroleum wax intermixed with resins, asphaltic material, and crude oil. They may also contain a variety of foreign materials such as sand, silt, water, various metal oxides, sulfates and carbonates of iron. barium, and calcium. The petroleum waxes deposited in flow strings usually consist of both a "hard" and a "soft" wax fraction. These waxes are largely aliphatic hydrocarbons with smaller amounts of aromatic and naphthenic compounds. Nathan' has classified the hard and soft wax fractions. The aliphatic hydrocarbons present are those of high molecular weight with high melting points. Reistle3 pointed out that these high molecular weight compounds first separate from the oil due to a sharp decrease in solubility as the melting point increases. The identification of the resins and asphaltic materials rests, at present, on an arbitrary solubility procedure. Under certain conditions, materials which are insoluble in pentane (ASTM D-893) are defined as resins and asphalts. Subgrouping of these materials is made on decreasing solubility in benzene and carbon disul-fide. Shock' found some correlation be-tween the solvent response and the pentane insoluble content of paraftins: higher pentane insoluble fractions are less soluble in any of the commonly used commercial solvents. PARAFFIN CONTROL METHODS The methods used in oil fields to prevent and remove paraffin accumulations can be grouped into four general classes: (1) operative methods, (2) physical methods, (3) chemical methods, and (4) combination of any of these. Operative methods attempt to prevent the formation of paraffin deposits while the other methods are concerned primarily with the removal of these deposits. Plastic coated pipe has been used for a number of years to prevent cor- rosion in wells, and in manv instances paraffin deposits have -been greatly reduced. Field observations have indicated that plastic coated pipe not only reduced paraffin accumulation but in some cases eliminated deposition completely; however, data are needed to demonstrate the relative effectiveness of plastic materials. Deposition Apparatus The pipe used to determine the effect of velocity on rates of deposition was %- and 2-in. nominal diameter, and 5 ft in length. Steel, butyrate, rigid PVC, kralastic resin-type plastic pipes, epoxy coated pipe, PVC lined glass fiber pipe, and aluminum pipe were tested. Steel pipe was used as a control. Fig. 1 is a schematic diagram of the apparatus showing the relative position of the separate units making up the equipment. In order to facilitate the installation and removal of the test pipes in the apparatus, O-ring seals capable of sustaining pressures of 50 psi were provided at each end. Test pipes were submerged in a cold water bath maintained at or below room temperature by circulating water through copper cooling coils packed in ice. A hot water bath equipped with immersion-type heaters, stirrers, and a thermoregulator was used to maintain the temperature of the oil prior to introduction into the piping manifold. The capacity of the oil reservoir was 30 gal. A 33-gal/min centrifugal pump, capable of producing turbulent flow velocities in the test pipes, was used to circulate the oil through the system when using %-in. pipe; and a 70-galjmin centrifugal pump was used in later tests using 2-in. pipe. A by-pass arrangement made it pos-

By C. S. Barrett, D. B. Masson

Martensitic transformations have been found in AgCd both upon cold-working at room temperature and cooling to lower temperatures. The crystal structures of the transformation products were found to be close-packed hexagonal in the first case and or-thorhombic in the latter. The transformation characteristics also were studied. Similar treatment of AuZn alloys failed to yield any transformation. THE literature on martensitic transformations of body-centered cubic metals and alloys indicates widespread instability of this structure at low temperatures, a tendency which merits further study. The body-centered cubic ß-phase of CuZn, for example, when it contained less than 42 wt pct Zn, was found by Greninger and Mooradian' and others' to transform on cooling to subzero temperatures to a phase that was tentatively considered to be tetragonal. Further work by Massalski and Barrett" demonstrated that cold work at low temperatures causes a partial transformation of ß CuZn of higher Zn content. The structures of the strain-induced transformation products were found to be different from those induced by simple cooling. Another well-known martensitic transformation among body-centered cubic phases is that of ß AuCd, first studied with X-rays by Olander,' then very thoroughly by Chang and Read.5,6 Here again transformation was found to occur both as a result of cooling and of strain. The alkali metals Li and Na, as well as certain Li-Mg alloys, also undergo transformation from their normal body-centered cubic structure, both on cooling and on cold-working. The phase AgCd, the subject of the present report, should be expected to behave quite similarly to CuZn for a number of reasons. It is the chemical analogue of CuZn, silver being directly below copper and cadmium directly below zinc in the periodic table. The size factors (percent difference in size) of the atoms, possibly a consideration in the stability of the ß-phases, are +3.1 in AgCd and + 4.2 in CuZn. Likewise the relative electronegativities of the two pairs of metals are about the same, CuZn possessing an electronegativity difference of 1.0 and AgCd one of 0.8. These values are from a table of electronegativities given by Darken and Gurry." The phase diagrams of the two systems around 50 atomic percent are similar, both possessing a disordered body-centered cubic phase, ß, at high temperatures and an ordered bcc phase, ß, at room temperature; however, the ß and ß' phases of AgCd are separated by a hexagonal phase, [, stable in the range 220-440oC, which has no analogue in CuZn. There has been confusion in the literature as to the structures of the ß' and [-phases. The phase diagram in the ASM handbook'" has the structures of the two phases interchanged; however, Hansen" reports the correct relative positions and Muldawer" verified that ß', the low-temperature phase, is body-centered cubic. Work by the present authors also

Jan 1, 1959

By Milton E. Wadsworth, John N. Ong, W. Martin Fassell

The temperature and oxygen concentration dependence on the reaction of sphalerite in oxygen at pressures from 6 to 640 mm Hg have been investigated in the temperature range 700° to 870°C. Sphalerite has been found to oxidize linearly over this entire temperature and pressure range. At higher rates, considerable self-heating was observed. The dependence of the oxidation rate on the oxygen concentration may be expressed by: Rate = k' where k' is the specific rate constant and 0 = K1[O2]/(1 + KI[O2]), where K1 is the equilibrium rate constant for the adsorption of oxygen on sphalerite. Values of the activation energy and the enthalpy of adsorption were found to be 60.3 and —59.6 kcal per mol, respectively. Data have been presented that indicate conditions under which either a sulphatizing or an oxidizing roast may be obtained. ROASTING processes have been employed in the metallurgy of a great number of basic metals in use today. Until recently, however, little attempt has been made to deduce the fundamental mechanism by which oxidation takes place. Structural changes upon oxidation have been investigated1 = and thorough work has been performed with regard to the reaction products and the thermodynamics of the oxidation reactions. The objective of this investigation was to determine the rate of oxidation of sphalerite and to apply the absolute reaction rate theory in the theoretilcal interpretation of the experimental results." "O Description of Apparatus The apparatus contains the following features: 1—a furnace with gas system, 2—an autographic weighing system, and 3—a temperature control system. Furnace With Gas System—The furnace was mounted by a yoke on each end and was free to travel up and down on steel guide rods, permitting the introduction and removal of samples from the apparatus with minimum difficulty. The furnace was heated by three sections of Kanthal wire wound externally on a zirconia tube and insulated with Fiber-frax. Pure gases or mixtures of gases were introduced into the lower end of the furnace through two flowmeters, a mixing chamber, and a gas-tight sparger, Fig. 1. The gaseous products of the reaction and the unused gases were prevented from escaping to the atmosphere by maintaining a small negative pressure on the system. This procedure permitted air from the outside to enter through the small an-nulus around the quartz suspension fiber and prevented the escape of the internal gases. Autographic Weighing System—The autographic weighing system consisted of an adapted gold balance, a photoelectric circuit, and a weight recorder, Fig. 2. The sample was suspended from one end of the balance beam by means of a platinum chain outside the furnace and a long thin quartz fiber on the inside of the furnace. On the other end of the balance beam, the necessary weights were added to counterbalance the sample. In addition, a calibrated chain was added to the balance which was linked directly to the weight recording unit. Control was effected by means of a photoelectric circuit." A parallel beam of light from a strong source was directed onto a small front-surfaced aluminum mirror mounted in the middle of the balance beam and then to a front-surfaced mirror mounted on the ceiling of the room. The beam was then reflected onto a front-surfaced right prism at a distance of 9 ft from the balance

Jan 1, 1957

By E. H. Dix

All commercial aluminum contains small percentages of copper, iron, and silicon as unavoidable impurities. The purest metal obtainable commercially, special grade high purity ingot, contains a maximum of 0.50 per cent. impurities of which the usual minimum amount of copper is 0.01 per cent.; silicon, 0.12 per cent.; and iron, 0.20 per cent. This grade is too costly for most purposes. The two standard grades, Nos. 1 and 2, containing a minimum of 99.0 and 98.0 per cent. aluminum, respectively, are more generally used. Other grades of secondary aluminum often contain as high as 3 or 4 per cent. of impurities, which include 1 per cent., or more, of zinc. Specifications for high-grade aluminum-casting alloys generally allow a maximum of 1.7 per cent. for total impurities. The S. A. E. Specification No. 33, which is intended to cover alloys made from secondary aluminum ingot, gives the iron maximum as 1.5 per cent. and the maximum for silicon (including manganese and tin) as 0.75 per cent. The effect of even relatively small amounts of impurities on the physical properties of ingot aluminum is shown by the following cornparison of two lots of aluminum, which may be taken as representative of special grade and grade No. 2 ingot, respectively. AnalysEs Special Grade, Gbade No. 2, Per Cent. PeR CBnt. Copper................................. 0.01 0.32 Silicon................................. 0.12 0.32 Iron................................... 0.42 0.82 Aluminum.............................. 99.45 98.54

Jan 1, 1923