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By A. F. Giamei, E. J. Freise

A discussion of the various factors affecting the accuracy of volume fraction determination by the direct comparison X-ray diffraction method is presented. To minimize errors introduced by nonrandomization effects such as preferred orientation and large grain size, as well as errors introduced by statistical effects, an iterative mathematical analysis is introduced. This analysis is applied to all observable diffractio~ spectra from a given specimen by means of computer techniques and is statistically superior to the standard direct comparison technique which utilizes only one or tm sets of intensity spectra. The computer program also presents a graphical interpretation of- the results which enables the investigator to visualize and readily assess the scatter in volume fraction estimates caused by deviations from randomness. Finally, the iterative analysis is applied to experimental data collected from a series of plain carbon steels in both the as-received and spheroidized conditions to determine the volume fraction of cemen-tite present in each case. The results show markedly good agreement with chemical analyses for all spheroidized specimens. In theory, quantitative X-ray diffraction is a power-ful analytical technique for precise determination of the volume fractions of various phases present in a multiphase poly crystalline aggregate. There are two generally used methods; both utilize the fact that the intensity of a diffraction line of a particular phase is a function of volume fraction of that phase present in the aggregate. The more common method is the so-called internal standard technique where a known amount of standard substance is mixed with the aggregate containing the unknown. The resulting ratio of the intensity of a particular diffraction line of the unknown to the intensity of a diffraction line from the standard is used to find the weight fraction of unknown material by reference to the intensity data obtained from a previously prepared set of standards containing the same amount of standard material. The details of this technique are outlined in standard works on X-ray diffraction.' The disadvantages of the technique are that it requires the use of powder specimens and that the powder mixture must be homogeneous near the surface to the maximum effective beam depth. The alternative technique is the direct comparison method in which the ratio of the intensity of a diffraction line of a phase in the aggregate to the intensity of a second-phase diffraction line yields the ratio of the volume fractions of each phase present. This method has been applied most extensively to the determination of the percentage of retained austenite in martensitic steels and to determining the amounts of hcp and fcc allotropic modifications in pure cobalt5 and the amounts of hexagonal and rhombohedra1 modifications in graphite.8 This method is applicable to bulk as well as powder aggregates and is the technique which will be considered in the following text. It is the purpose of the present communication to show that by combining the results of X-ray diffrac-tometry with the use of high-speed digital computers the results of the direct comparison quantitative X-ray analysis technique can be optimized by using all of the data available on a diffraction pattern. THEORETICAL DISCUSSION In optimizing any quantitative X-ray diffraction experiment, the problem of accuracy vs time to collect and analyze the experimental data arises. For any method to be practical, it is required that both experimental and analytical procedures are reasonably short. In most of the previous work performed by the direct comparison method, intensity data from only one or two sets of peaks were used to calculate the volume fraction of phases present in the aggregate. Consequently, rather long-time experimental measurements are required to assure that the intensity data are sufficiently accurate to justify the use of one or two sets of data. By using computer techniques to analyze the experimental data it becomes feasible to use all of the available data on a diffraction pattern. By so doing, the time spent in measuring any one diffraction maxima can be appreciably reduced. Although this results in poor counting statistics for any one maxima, the number of data points available for analysis is greatly increased. Based on the above discussion, it will be assumed that a continuous scanning counter-diffractometer technique will be used to collect intensity data from a two-phase mixture. The integrated intensity of the ith diffraction line from the a phase in the aggregate is given by:'" where is the volume fraction of the a phase, The various quantities in Eq. [la] are angular independent while those in [lb] depend on the hkl spectrum of a particular phase. The meaning of the individual quantities in Eqs. [la] and [lb] are given in Appendix 1. It is convenient at this point to outline briefly the factors which will affect the measured intensity of any one hkl spectrum. a) Extinction effects arise from two independent experimental conditions. Primary extinction arises from a high degree of crystal perfection and results in spectra having lower intensity than predicted by Eq. [I]. Any treatment, such as powdering, which reduces

Jan 1, 1968

By Henry Mulryan

The largest and purest known deposit of diatomite is being actively mined and processed 3 1/2 miles south of Lompoc, Santa Barbara County, Calif., by the Johns-Nlanville Products Corporation. The workings cover 4000 acres, the depth of economically recoverable diatomite being 1000 ft. (Fig. 1). Lompoe, a community of 2500 population, is situated in the Santa Ynez River Valley 10 miles inland from the Pacific Ocean. It is 44 miles

Jan 1, 1938

By Henry Mulryan

The largest and purest known deposit of diatomite is being actively mined and processed 3 1/2 miles south of Lompoc, Santa Barbara County, Calif., by the Johns-Nlanville Products Corporation. The workings cover 4000 acres, the depth of economically recoverable diatomite being 1000 ft. (Fig. 1). Lompoe, a community of 2500 population, is situated in the Santa Ynez River Valley 10 miles inland from the Pacific Ocean. It is 44 miles

Jan 1, 1938

By B. W. Gandrud

WET-PROCESS coal-washing tables as we know them today have been in use in this country for approximately 25 years. The literature records only a few table installations worthy of note prior to adoption of the present-day differential-motion table. According to Phillips,' six Campbell bumping tables were being operated by the St. Bernard Coal Co., Earlington, Ky., in 1893. As late as 1923, according to Richardson, 72 such tables were in operation in the Rosedale washery of the Cambria Steel Co., at Johnstown, Pa. Bumping tables probably were not used to any considerable extent except in the plant at Earlington, and at two or three plants in Pennsylvania, but they may be considered as forerunners of the present-day coal-washing table. The transition from bumping tables to the type of tables now in use signalized a revolutionary change iii table design. The advantages of the new design over the old were so outstanding as to make its adoption inevitable. BUMPING TABLES Bumping tables, as the name implies, utilized a bumping action for conveying the refuse and discharging it over the refuse end. The tables were hung from rods attached to overhead supporting beams. A shaft and cam arrangement at one end of the table served as ,the actuating mechanism and imparted to the table an endwise, back-and-forth, swinging motion. A bumping block was fixed in the proper position at the shaft end, so that the table would strike against it at the end of each backward swing. The hanger rods or stirrups were so adjusted as to give the table a slight uphill slope toward the refuse end; that is, the end next to the driving mechanism. The feed box was near the upper end of the table and designed to spread the mixture of coal and water over the width of the table. Wash water was added a short distance below the feed box. With the table in motion and coal mixed with water being fed to it through the feed box, a certain amount of stratification took place, depositing heavy refuse at the bottom of the bed in contact with the surface of the table. Constant bumping and a certain amount of

Jan 1, 1943

By Clarence Seyler

THE technical difficulties of cutting thin sections of coal for examination by transmitted light have hitherto restricted the investigation of the important subject of the microstructure of coal to the few possessed of the requisite skill and time. Apart from this, the method fails with anthracites and other coals rich in carbon, owing to the opacity of the material. Occasional use of the method of polishing a surface, with or without etching, has been made, but it was not until Winter1 published an account of his results that attention was seriously directed to the method. In May, 1923, a specimen of dull anthracite came into my hands; I tried Winter's method on it and the presence of megaspores and other vegetable structures became clearly visible. A preliminary notice was published by me;2 but I soon abandoned the use of Schulze's solution having found that a mixture of chromic and sulfuric acids gave far better results. In the meantime Turner and Randall, in America, had independently developed the method of flame etching, as applied to anthracite, with great success. I have spent a year studying the method of chromic etching, which gives excellent results with bituminous coals and cannels, as well as with anthracite. For anthracites, I have used the chromic method and Turner's method of flame etching, whichever was the more convenient or as a check one on the other. The polishing is done, according to metallurgical practice, by the use of a polishing machine and successively finer emery paper, followed by polishing on cloth moistened with a suspension of levigated green oxide of chromium, and a final rubbing on "selvyt" (a cotton velvet polishing cloth) moistened' with alcohol. The polished sample is examined by reflected light with a 2/3 and 1/6 in. objective. Bituminous coals usually show considerable structure, and even anthracites show it faintly in places. The sample is then etched by immersion in a boiling solution made by adding 10 c.c. of concentrated sulfuric acid to 30 c.c of a saturated solution of chromic acid; enough water is then added to dissolve

Jan 3, 1925

THE Institute conducts jointly with the American Society of Civil Engineers, American Society of Mechanical Engineers and American Institute of Electrical Engineers, certain activities as listed below, and is joint owner with them of certain properties situated at 29 West 39th Street in New York City.

Jan 1, 1946

By H. A. Meyerhoff, R. J. Colony

Deposits of iron are widely scattered in the folded Cretaceous rocks and the associated igneous intrusives of Puerto Rico. Most of them are too small for commercial development, but a few have aroused some scientific and economic interest, among them the large body of residual limonite at the west end of the island near Mayagüezl-6 (Fig. 1) and the mixed hematite and magnetite deposit on the southern slopes of the Sierra de Cayey, about four miles north of Arroyo.7"9 Neither of these orebodies has been developed, nor have investigations of the widely distributed deposits of magnetite, which include all the remaining occurrences of iron deserving of economic consideration, proceeded beyond the exploratory stage. With the possible exception of the mixed deposit near Arroyo, the magnetite is directly associated with andesitic and dioritic intrusives, which invade the Cretaceous rock section, and the bulk of it, occurring in calcareous sediments, is clearly of contact-replacement origin. The small deposit on Rio Portugües, north of Ponce, is found in a limestone band near its contact with an andesite dike.10,11 Two deposits of unde-

Jan 1, 1935

By H. A. Meyerhoff, R. J. Colony

Deposits of iron are widely scattered in the folded Cretaceous rocks and the associated igneous intrusives of Puerto Rico. Most of them are too small for commercial development, but a few have aroused some scientific and economic interest, among them the large body of residual limonite at the west end of the island near Mayagüezl-6 (Fig. 1) and the mixed hematite and magnetite deposit on the southern slopes of the Sierra de Cayey, about four miles north of Arroyo.7"9 Neither of these orebodies has been developed, nor have investigations of the widely distributed deposits of magnetite, which include all the remaining occurrences of iron deserving of economic consideration, proceeded beyond the exploratory stage. With the possible exception of the mixed deposit near Arroyo, the magnetite is directly associated with andesitic and dioritic intrusives, which invade the Cretaceous rock section, and the bulk of it, occurring in calcareous sediments, is clearly of contact-replacement origin. The small deposit on Rio Portugües, north of Ponce, is found in a limestone band near its contact with an andesite dike.10,11 Two deposits of unde-

Jan 1, 1935

By M. A. Mahtab, T. M. Yegulalp

This paper presents the development and application of an approach for clustering fracture orientation data. Data are projected on the surface of the unit upper hemisphere and the clustering approach is applied in three steps: (1) randomness test and identification of dense clusters, (2) estimation of cluster statistics, using Bingham distribution, and (3) rejection of extremal data based on Chauvenet's criterion.

Jan 1, 1982

By Frederic Becket

IN a recent article,1 which described the softening effect of columbium in plain high-chromium steels, the authors stated that their investi-gations had shown columbium to be also a particularly valuable inhibitor of intergranular corrosion in steels of the 18 per cent chromium, 8 per cent nickel type. It is the purpose of the present paper to record some of the results obtained through the introduction of columbium to the austenitic chromium-nickel steels. The damaging effects of this type of corrosion have become so widely known as to restrict considerably the applications of the steels under consideration, and therefore there is little question of the importance of the goal to be attained. Numerous contributions concerning the susceptibility of the aus-tenitic chromium-nickel steels to intergranular corrosion have appeared during the past few years, and among others who have dealt construc-tively with the subject are such well-known authors as Strauss and Houdremont of Germany, Hatfield of England, and Bain in the United States. Different theories have been propounded as to the cause of intergranular corrosion, and various remedial measures have been proposed, the majority of which involve the use of addition agents. Titanium is the addition agent at present most generally employed, as suggested by Houdremont and modified as described by Bain, Aborn and Rutherford.2 Little has been published on the effects of holding these steels for long periods at the relatively lower temperatures in the presence of

Jan 1, 1934

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 James A. Lewis

It is the purpose of this paper to show the importance of sand characteristics, when combined with other physical data, in evaluating production obtained by secondary recovery operations, and to indicate the benefits to be gained from the application of these principles to primary production.

Jan 1, 1942

By R. A. L. Black, J. E. Jennings

The problems of slope stability in open cast mines are examined. A criterion, the instantaneous stripping ratio, is suggested for use in the design of pit slopes and as an index of control at all stages of the exploitation of the orebody. This criterion may also be related to safety and to the maximizing of profits. Two approaches to safe design of slopes, one from the point of view of soil mechanics and the other from the point of view of rock mechanics, are described and critically compared. The effect on slope stability of the regional tectonic stress field is discussed. Explanation is given of the application of the Terzaghi effective stress concept to problems in both soil and rock environments, including possible effects when borehole deformation techniques are used to measure stresses in rock in situ. A company embarking on open cast mining is faced with two basic questions: 1) will the venture be profitable and 2) can it be carried out with safety? The two questions are obviously interrelated because both depend upon the slope angles adopted for the pit. The cost of open cast mining depends largely upon the stripping ratio, defined as the volume of overburden that must be removed to the volume of ore recovered. The steeper the slope angles, the more favorable the stripping ratio, but the stability of the slopes, and therefore the safety of men and materials in the pit, require that the angles be made relatively flat. Consequently, the design depends upon a compromise: the slopes must be steep enough to result in economical mining and flat enough to ensure safety. Today there is a world trend towards deeper mining by open cast methods. This is mainly due to the higher cost of underground mining and the lower cost of open excavation resulting from the introduction of large modern earth and rock-moving machinery. Deeper open cast mining has led to a very great increase in the volumes of wasted overburden, and much thought is being given to the considerable economic benefits which would result if pit slopes could be made steeper by even one or two degrees. The result has been an increasing interest in research into slope stability problems in the expectation that the application of scientific principles will provide solutions leading both to economies and to more predictable operation of the mines. In at least four places, the U.S., Australia, Western Germany and Southern Africa, comprehensive investigations are at present in progress, and it is the object of this paper to review some of the more important aspects of these programs. RELATION BETWEEN ECONOMY OF OPERATION AND SLOPE ANGLES The main object of any industrial enterprise in a free economy is to make a profit. In mining, where profits must be made from a wasting capital asset, a further definition of the profit motive is imposed, namely that the economic aim should be to maximize the total possible profit. But since profits deferred for a number of years are not as valuable as profits that are immediately available, it is usual to discount deferred profits at some rate of interest which reflects their current or present value in the hands of the investor. Thus, in mining the logical aim can be defined more closely still: to maximize the present value of the total future profits. In commercial terms the present value represents the market value of the operation as a going concern. Many factors enter into the forecast of current and future profits. They include the volume of production, the price of the salable product and the cost of production. Current profits can be estimated with reasonable accuracy by the operating engineers; but it is the task of economists and management to assess future trends in the mineral markets and in the economy as a whole, and together with the engineers, they can then estimate the future cost and profitability of the mining operations. In open cast mining, the rate of ore production once decided on remains a virtually constant factor unless a major change in the capital structure of the mine is made. But one factor over which the operator has a considerable measure of control is the ratio of the volume of ore mined to the volume of waste over-

Jan 1, 1963

By O. W. Ellis

The question of the influence of gases upon the properties of copper has received the attention of a number of investigators, among whom Sieverts,' Iwase,2 Lobley and Jepson3 stand preeminent. Solubility of Gases in Copper Sieverts and Iwasé concerned themselves with the solubility of a variety of gases in the metal in the solid and liquid states. They determined the absorption coefficients of these gases and in all cases found a sharp change in solubility at the melting point of the metal. In this respect they disagree with Lobley and Jepson, who have based their opinions upon the appearance of small ingots of the metal which had been fused in an atmosphere of one or other of three gases and had then been rapidly cooled, while surrounded by gas, to the freezing point (rate—possibly 30" to 60" C. per sec.). The ingots that had been fused and cooled under nitrogen and carbon monoxide were free from blowholes and it was assumed that these gases were not absorbed in amounts much in excess of those which would dissolve in the solid metal; the ingots similarly treated under hydrogen were full of blowholes and it was assumed in this case that gas was ejected on solidification of the copper. The effect of varying the rate of freezing upon the character of the test ingots was not examined by these investigators; otherwise, it is felt, their views might have been subject to modification. Sieverts' most important contribution is that the solubility of a gas in any metal is proportional to the square root of its pressure or concentration. Knowing then the absorption coefficients of the various gases in copper, it should be possible to determine the analysis of the

Jan 1, 1929

By Magnus Troilius

SINCE the discussion on steel rails in America has forcibly drawn attention to the value of chemical analysis, if not as a necessary stipulation, at least as a guide to control the usual mechanical tests, some doubt has been thrown upon the accuracy of the analytical results obtained by different chemists. To any one having the least acquaintance with chemistry, it is quite clear that if exactly similar results are to be obtained from the same borings of steel, exactly the same methods must be used by the different analysts. Hence the necessity (if complications are to be avoided) of establishing what I may call standard or normal methods, to be used both by the inspectors and by the chemists at the works. Remembering that the application of chemistry to steelrail inspection is yet in its infancy, it is of great importance to possess a perfect acquaintance with the best methods in use. Being myself a grateful pupil of Professor Eggertz, of the School of Mines in Sweden, it occurred to me, two years ago, that I could not do better than start a laboratory of my own, and engage one of his pupils, Mr. Troilius, for the purpose of analyzing the steel borings from mechanically-tested rails, so that I might thus obtain without delay thoroughly accurate determinations. Moreover, in order to carry on the operations in perfect accordance with the methods used at the steel works in England and Germany, where I had to control the manufacture, I deemed it desirable to allow Mr. Troilius to go through a course of training at these works; and I gladly seize this opportunity of expressing my grateful acknowledgments to several works in England and in Germany for affording every facility for such an exchange of information as mas found necessary in arriving at the best analytical methods to be used.

Jan 1, 1882

By O. W. Ellis

The question of the influence of gases upon the properties of copper has received the attention of a number of investigators, among whom Sieverts,' Iwase,2 Lobley and Jepson3 stand preeminent. Solubility of Gases in Copper Sieverts and Iwasé concerned themselves with the solubility of a variety of gases in the metal in the solid and liquid states. They determined the absorption coefficients of these gases and in all cases found a sharp change in solubility at the melting point of the metal. In this respect they disagree with Lobley and Jepson, who have based their opinions upon the appearance of small ingots of the metal which had been fused in an atmosphere of one or other of three gases and had then been rapidly cooled, while surrounded by gas, to the freezing point (rate—possibly 30" to 60" C. per sec.). The ingots that had been fused and cooled under nitrogen and carbon monoxide were free from blowholes and it was assumed that these gases were not absorbed in amounts much in excess of those which would dissolve in the solid metal; the ingots similarly treated under hydrogen were full of blowholes and it was assumed in this case that gas was ejected on solidification of the copper. The effect of varying the rate of freezing upon the character of the test ingots was not examined by these investigators; otherwise, it is felt, their views might have been subject to modification. Sieverts' most important contribution is that the solubility of a gas in any metal is proportional to the square root of its pressure or concentration. Knowing then the absorption coefficients of the various gases in copper, it should be possible to determine the analysis of the

Jan 1, 1929

By F. H. Daniels

IN this, paper it is my intention to, call your attention to* a few of the many producers using blast, now, in common use in Sweden, and also those constructed by the Washburn & Moen Manufacturing Company at their Quinsigamond Works. During a prolonged stay in Sweden the writer had an opportunity

Jan 1, 1881

By Magnus Troilius

INTRODUCTION BY C. P. SANDBERG. SINCE the discussion On steel rails in America has forcibly drawn attention to the value of chemical analysis, if not as a necessary stipulation, at least as a guide to control the usual mechanical tests, some doubt has been thrown upon the accuracy of the analytical results Obtained by different chemists. To any One having the least acquaintance with chemistry., it is quite clear that if exactly similar results are to be obtained from the same borings of steel, exactly the same methods must be used by the different analysts. Hence the necessity (if complications are to be avoided) of establishing what I may call standard or normal methods, to be used both by the inspectors and by the chemists at the works. Remembering that the application' of chemistry to steel-rail inspection is yet in its infancy, it is of great importance to possess a perfect acquaintance with the best methods in use. Being myself a grateful pupil of Professor Eggertz, of the School of Mines in Sweden, it Occurred to me, two. years ago, that I could not do better than start a laboratory of my. own, and engage One of his pupils, Mr. Troilius, for the purpose of analyzing the steel borings from mechanically-tested rails, so that I might thus Obtain without delay thoroughly accurate determinations. Moreover, in Order to carry on the, operations in perfect accordance with the methods used at the steel works in England and Germany, where I had to control the manufacture, I deemed it desirable to allow Mr. Troilius to go through a course of training at these works; and I gladly seize this opportunity of expressing my grateful acknowledgments to several works in England and in Germany for affording every facility for such an exchange of information as was found necessary in arriving at the best analytical methods to be used.

Jan 1, 1882

By Earl S. Bardwell

The determination of suitable and safe annealing temperatures is one of the most important problems arising in the operation of a copper rolling mill. Certain of the larger mills have worked this problem out for themselves and in these mills the operation has become more or less standardized. In some of the mills pyrometers are used to measure the temperature of the annealing furnaces and careful watch is kept to see that overheating does not take place. In a considerable number of the mills, however, dependence is placed entirely on the judgment of the operator. The almost total lack of literature bearing on this subject seems sufficient warrant for the publication of this paper. ' The discussion of this subject naturally divides itself into two parts: (1) The effect of annealing temperature on physical properties; and (2) changes in the microstructure of refined copper due to cold rolling and annealing. I. The Effect of Annealing Temperature on Physical Properties For the purpose of investigating this phase of the subject six test bars were selected, varying in oxygen content between the limits of 0.036 and 0.070 per cent. The chemical composition of each of these test bars was as follows: Bar Number 1 2 3 4 5 6 Copper + silver...... 99.95 99.92 99.945 99.94 99.95 99.93 Oxygen.............. 0.041 0.070 0.046 0.050 0.036 0.058 As + Sb............. 0.0038 0.0038 0.0038 0.0038 0.0031 0.0031 The bars were heated in an electric muffle to about 1,650" F. and rolled into rods. The rods were annealed, pickled, and drawn to No. 12 B. & S. gauge wire. The wire which was to be used for the annealing test was cut into 38-in. lengths and each length made into a coil 6 in. in diameter. The separate coils were marked so that they might readily be identified

Jan 1, 1915

By Wayne C. Hazen, James K. Kindig

As the complexity of hydrometallurgical systems increases, it offers new opportunity for applications of solvent extraction. However, the high capital cost of mixer-settlers for large flow rates is a drawback to wide application in base metal recovery. This paper presents information on the use of cyclone separators in place of settlers with attendant significant reduction in capital cost. Various flowsheet possibilities for this development are discussed.

Jan 1, 1972