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By Robert T. Howard, Morris Cohen

IT has long been realized among metallurgists that a fast, reliable method for the quantitative determination of the percentage of microconstituents in an alloy would be of great benefit in studies of equilibrium and transformation in the solid state. For example, Polushkin1 has shown that the compositions of two coexisting phases in a a binary system at a given temperature may be calculated very simply with the aid of two alloys lying in the two-phase field if the relative amounts of the two phases in each alloy can be determined. Recently, Grange and Stewart2 have traced the course of the austenite-martensite reaction in a series of commercial steels by making visual estimates of the percentage of martensite formed as a function of cooling temperature. The correlation of mechanical properties with structure, a subject of wide-spread current interest, is likewise dependent upon quantitative microanalysis.3 Yet, there are very few investigations described in the metallurgical literature, wherein methods of quantitative microscopy are employed. Usually, the relative amounts of the microconstituents are estimated in a qualitative or semiquantitative way. The authors were faced with this problem some time ago in studying the kinetics of austenite decomposition. Several aspects of, this research could not be treated satisfactorily by other quantitative tools, such as specific volume,4 magnetic,5 dilatometric,6 electrical resistance7 or x-ray measurements.8 It became necessary to find an impersonal quantitative method that could be applied to microstructures. Fortunately, it was noted that geologists and petrographers had coped with quantitative microscopy to a considerable degree in their attempts to evaluate the mineral contents of rocks. A number of excellent articles were found on this subject, and since they appear to be unknown generally to many metallurgists, the first part of the present paper is concerned with a review of the literature in some detail. With this survey as a background, the authors have adapted the so-called methods of point-counting and lineal analysis to metallography, as described in the second part of the paper. Austenite-martensite structures were selected for illustration not only because they are important in many ways, but because such fine intermixtures are notoriously difficult to estimate visually. LITERATURE SURVEY Perhaps the earliest work on quantitative microscopic analysis goes back to Delesse9 (1848) who proved mathemati-

Jan 1, 1947

By D. P. Harris

This paper examines recent developments and work in progress on the application of quantitative methods and computers to the appraisal of the mineral resource potential of discrete areas by employing reconnaissance geological information and general economic relationships. The perspective of this paper might be that of a firm planning a regional exploration program or of a legislative body seeking to choose between several alternative actions on the basis of their impact upon the regional resources. In addition to this general survey and commentary, an example is presented of the use of geostatistical analysis and computer simulation to evaluate the economic mineral resources of the Seward Peninsula of Alaska.

Jan 1, 1969

By W. M. Tuddenham, R. J. P. Lyon

In many areas surrounding the orebodies in mining districts rocks have been bleached and altered by the ore-forming solutions and have been oxidized during later weathering processes. A number of the rock-forming silicates have been broken down to clay, sericitic micas and chlorites have been developed, and pyrite may be found hundreds of feet outside the economic limits of the orebody. These halos of altered ground are prime targets used by geologists in many districts to delineate promising sites for drilling. Both in the field and in the laboratory it is often difficult to map these mineralogical changes in the halos in detail without numerous petrologic examinations. The secondary minerals are generally fine-grained, and since conversion of one mineral to another is often progressive, many alteration processes have not proceeded to completion (feldspars to clay to sericite mica). Qualitative detection of these minerals is difficult; quantitative determination is frequently impossible.

Jan 12, 1959

By Reynold Q. Shotts

Nitric acid oxidation rate analyses of three coals, previously studied microscopically by the Bureau of Mines, revealed three components. Relative quantities agree with those found for the four components given by the Bureau and results are consistent with current ideas of coal constitution. Possible multi-component composition for bright coal and a reactivity-rank relation are suggested.

Jan 5, 1953

By Lester W. Strock

METALLURGISTS handling lead and zinc ores have long been familiar with the spectrograph as a routine analytical tool, as its earliest regular use by American industry was in controlling impurities of zinc metal and its alloys. This application has been extended to other metal industries on an extensive scale, accompanied by refinements of procedure to such an extent that a large part of some metals produced, especially magnesium, aluminum and steel, are checked only by spectrographic methods for conformity to specifications. The spectrographic analysis of ores and other poorly conducting powdered solids presents difficulties not encountered with metallic samples, which can be arced or sparked as self-electrodes or can be readily dissolved, so that their solutions can be analyzed, as in the American Society for Testing Materials standard methods for zinc and zinc-base alloys. Spectra of powdered solid samples can be prepared by using carbon electrodes provided with a crater of suitable size, into which the sample is packed. Ore samples and many other powdered solid materials usually analyzed in the chemical and metallurgical laboratory are more complex and varied in composition than samples of metals produced in large tonnages. More preliminary work therefore is usually necessary in devising a spectrographic method for analyzing a given type of powdered sample than for analyzing metal samples, in order to use that method with confidence. The knowledge that the standard samples and unknowns produce equivalent line intensities at equal concentration is the fundamental basis of any quantitative spectrographic method. On the other hand, powdered samples have an advantage over metals in that any desired number of chemical compounds can be mixed dry in any desired ratio to produce a synthetic standard. Experience has shown, however, that spectra of elements in finely divided compounds introduced into a standard in preparing a synthetic ore sample do not always behave in the electric arc in a manner that produces spectral line intensities similar to those observed at the same concentration in a natural mineral. In ore samples minor elements frequently are contained in the crystal lattice of larger particles of an abundant ore mineral. Their dissociation and volatilization from the sample into the arc then proceeds differently in the standard and sample, with resultant differences in intensity. During the past 10 years I have devised and applied several quantitative spectrographic methods for determining various elements in rocks and minerals in connection with studies on their geochemistry,1 but the incentive has gradually changed since the summer of 1940 to the specific practical problem of searching for domestic sources of rare and strategic metals. The

Jan 1, 1945

By F. Twyman

PART I.-QUALITATIVE, SPECTRUM ANALYSIS THOSE chemists (they are still greatly in the minority) who use the spectroscope, use it very often, and find it almost indispensable. As a means of detecting minute quantities of the metals it is unrivalled. A metal can be readily distinguished in the presence of any other element, compound, or mixture without the necessity of separation. The qualitative analysis of the metallic constituents of a substance, which, the spectroscope gives so easily, is a sure basis for planning a chemical analysis. As the determination of each element proceeds the purity of precipitates maybe checked as often as desired. If, possessing these advantages; the spectroscope has been neglected in general chemistry, it is not surprising that it was neglected in metallurgical chemistry; for many of the impurities which are of industrial interest, even when they are present in a metal or alloy in small quantities, are not then always easily detected by the examination of their visible spectrum. The history of the development of the art has been given in Bureau of Standards Scientific Paper No. 444.

Jan 1, 1928

By F. Twyman, D. M. Smith

THOSE chemists (they are still greatly in the minority) who use the spectroscope, use it very often, and find it almost indispensable. As a means of detecting minute quantities of the metals it is unrivalled. A metal can be readily distinguished in the presence of any other element, compound, or mixture without the necessity of separation. The qualitative analysis of the metallic constituents of a substance, which the spectroscope gives so easily, is a sure basis for planning a chemical analysis. As the determination of each element proceeds the purity of precipitates may be checked as often as desired. If, possessing these advantages, the spectroscope has been neglected in general chemistry, it is not surprising that it was neglected in metallurgical chemistry; for many of the impurities which are of industrial interest, even when they are present in a metal or alloy in small quantities, are not then always easily detected by the examination of their visible spectrum. The history of the development of the art has been given in Bureau of Standards Scientific Paper No. 444.

Jan 1, 1928

By John R. Wynnyckyj

Results of correlations between strength-development and sintering shrinkage occurring during induration are presented. A mathematical treatment of the shrinkage kinetics is, next, given and is based on the use of semi-empirical equations. The discussion stresses the significance of kinetic constants and activation energies in the assessment of iron ore concentrates for pelletizing and induration. Next, starting with the assumption that there is a need for parameters to characterize the iron-ore concentrates and relate these parameters to shrinkage-kinetic constants and balling behaviour, results of compaction measurements and pore structure characterization (mercury porosimetry) are presented and discussed.

Jan 1, 1977

By R. S. Shoemaker, D. L. Harris

Past investigations into the possibility of concentrating the low-grade iron ores of the Gogebic Range in Wisconsin have been hampered by the complex association of the constituent minerals. In part the problem arises from the fact that the iron occurs essentially as two minerals, hematite and goethite, having nearly the same chemical composition but exhibiting different physical properties. Individual grains of these minerals are usually so small that the ore must be ground to a size finer than 325 mesh if substantial liberation of the minerals is to be secured. Appraisal of beneficiation tests on this iron ore requires, therefore, some method of determining quantitatively the contents of constituent minerals in the various products of the beneficiation. Because of the chemical similarity of the two iron minerals, chemical analyses do not provide a means of differentiation. Although the minerals are different physically, they are both opaque and friable, and as the ore must be ground to a very fine size for liberation to be secured, quantitative microscopic methods of analysis are extremely difficult at best. In an effort to overcome these analytical problems, a quantitative X-ray diffraction analysis method has been developed at the University of Wisconsin for the research program on iron ore beneficiation.

Jan 5, 1955

By B. Barlin, G. A. L. Smith, I. J. I. Delaney

A method was developed to quantify the three mineral species, sphalerite, galena, and pyrite in seven concentrator products. Intermineral effects were studied and a statistical analysis was undertaken to assess the accuracy and reproducibility of the method. The method is both rapid and suitable for plant control purposes. Furthermore, it requires only semiskilled laboratory personnel to carry out all the analyses.

Jan 1, 1976

By D. T. Farnham

The shale used at the Renton plant of the Denny-Renton Clay and Coal Co. for the manufacture of vitrified paving brick occurs in a hill rising from 200 to 300 ft. above the level of the valley in which the plant is situated.

Jan 1, 1915

By E. H. Jr. Crabtree

THE productive area of asphalt-bearing sandstone in Missouri is near the Missouri-Kansas state line near Nevada, the county seat of Vernon County about 100 miles south of Kansas City. While produc-tion thus far has been confined to Vernon and Barton counties, there are known deposits in adjacent counties. The area is served by four rail-roads: the Missouri Pacific, the Kansas City Southern, the Missouri-Kansas & Texas, and the St. Louis & San Francisco. The plant of the Reliance Rock Asphalt Corporation is in Vernon County, about 5 miles west of Nevada, at Ellis, a flag station on the Missouri, Kansas & Texas Railroad. A siding has been built to the plant so that the finished product can be loaded directly into railroad cars. The property consists of a lease of 240 acres in one block. All portions of the property not required for quarrying or processing the asphalt-bearing sandstone are used for farming by the fee owner. The entire tract is very flat so that there are no transportation difficulties from quarry to plant.

Jan 1, 1935

By J. B. Newsom

IN the Indiana limestone district, some 50 or 60 per, cent of the merchantable stone in a quarry opening is waste, and only about 40 or 50 per cent of the stone from the opening is finally sold. So long as the present system of quarrying is used, the wastes measured and reported in this paper will continue. Comprehensive development of an entirely different method of quarrying, using wire saws for cutting, promises great improvement. Some of the savings to be expected are pointed out in the following pages. No attempt has been made to measure losses due to variations and natural flaws in the stone, since these vary greatly in different quarries, and accurate measurement would be difficult. The wastes that have been measured account for about 30 per cent of the total ledge, which leaves 20 or 30 per cent chargeable to unmeasured sources of loss.

Jan 1, 1932

By P. F. MINISTER

AT Lime Spur, Mont., the East Butte Copper Mining Co. has been quarrying limestone for twenty years. The quarry is beside the Northern Pacific R. R. in the Jefferson River canyon, 4 ½ miles east of Cardwell, at Lime Spur, Montana. HISTORY This quarry was opened early in 1900 by Dan Morrison of Whitehall, the discoverer of the Morrison cave, to supply a demand for smelter flux. Limestone was sold to the Pittsmont smelter of The East Butte Copper Mining Co. and to the Butte Reduction Works. As no particular effort was made at the quarry to select the rock that delivered to the smelters was unduly high in magnesia and impurities. The East Butte com¬pany, therefore. Bought the quarry. in 1909 and confined operations to the high-grade beds in order to supply rock of the desired purity for its own smelter and the Butte Reduction Works until the latter shut down. It also developed a market for some of its rock with the sugar factories. The latter market increased until in later years all rock, larger than 4 in. in size over a bar grizzly, was being shipped to the sugar factories, and the rock smaller than 4 in. was being used as a flux in the blast furnaces at the Pittsmont smelter. In 1924, the East Butte concluded a contract with the Anaconda company for the treatment of its ores, and the Pittsmont -smelter -was shut down: which made the minus 4-in. rock a useless by-product. Since there was not enough revenue in the sugar rock alone and also because of limited waste room it became necessary, if Lime Spur was to continue to operate, to increase- the proportion of plus 4-in. rock and to develop a market for the minus 4-in.

Jan 1, 1930

By Dwight Farnham

Description of Quarry THE shale used at the Renton plant of the Denny-Renton Clay Coal Co., for the manufacture of vitrified paving brick occurs in a hill rising from 200 to 300 ft. above the level of the valley in which the plant is situated. The shale deposit, which is of unknown thickness pitches about 10° to the southeast. The 150-ft. face worked extends approximately east and west, so that the clip, as shown by the photograph, is to the left and into the hill. The shale is overlain with about 50 ft. of gravel, 70 ft. of clay, and 30 ft. of mixed loam and gravel, making altogether from 125 to 150 ft. of overburden. Disposal of Overburden The overburden is removed by sluicing. For this purpose a No. 2 Joshua Hendy giant is used, throwing a 12-in. stream', and having 60 lb. pressure at the nozzle. The water is drawn through an 8-in. pipe from Cedar river, about 1,000 ft. distant, by means of a Worthington four-stage centrifugal pump, direct connected with a 100-h.p. motor placed just south of the factory, and 1,500 ft. from the nozzle This plant handles the material satisfactorily to a height of about 75 ft. above the level of the top of the shale. When the higher levels are worked, an auxiliary plant consisting of a four-stage Byron Jackson centrifugal pump with a 100-h.p., belt-connected motor, is thrown into the system. This plant is situated on top of the shale and can be discerned at the extreme right of the trestle work in Fig. 1.

Jan 9, 1914

Discussion of the paper of DWIGHT T. FARNHAM, presented at the Pittsburgh meeting, October, 1914, and printed in Bulletin No. 93, September, 1914, pp. 2357 to 2364. DAVID T. DAY, Washington, D. C.-Do you know anything about the character of that clay as to organic matter? H. RIES, Ithaca, N. Y.-No; it is a dark brownish clay, sandy in its nature. The brownish coloring is probably due to organic matter. Some lignite is also present. DONALD W. Ross.*-I have worked at the plant under consideration. I have not seen Mr. Farnham's paper; but in answering the question as to the organic matter, I might say there is practically no organic material scattered through the shale. There are, however, several layers of carbonaceous shale and rather low-grade coal interbedded with the formation. There are two very serious drawbacks-one which threatens to shut down the plant and another which merely means the expenditure of money. The first is taking care of the sediment from the washing away of the overburden. The government is doing extensive work at different points about Lake Washington with a view to creating a fresh-water harbor for Seattle. I understand that they keep at the Denny-Renton people to keep the channel of Cedar River clear. The Denny-Renton Co. can hardly help filling up the channel so long as they continue their hydraulic work, so this is probably one of their most serious problems. The other is this: There is a large percentage of what I should call micaceous shale or sandstone-a sandstone which contains a large amount of light-colored mica. Of course only a limited amount of this can be used in the manufacture of paving brick. As they shoot down the bank after the overburden of gravel and loam is washed away, these large boulders of micaceous sandstone come down. The strata have apparently been crushed where the clay pit is located so that the exact formation cannot be readily determined. These pieces of sandstone, 5 or 6 ft. in diameter, have to be blasted and removed from the shale. They bother both in the open pit and in the tunnel mining. In the tunnel mining of the shale blocks frequently cover the holes in the roof of the tunnel through which the shale is loaded into cars.

Jan 4, 1915

By Robert B. McCormick

THE major use for quartz crystal is in the manufacture of radio oscillator plates and telephone resonator and filter crystals. Quartz crystal is also cut and polished as a semiprecious gem stone, particularly in the colored varieties (amethyst, Brazilian topaz, and others), and often is carved into various objects of art. Prisms, wedges, lenses and other optical parts often are made of quartz crystal, usually for special- purpose instruments. Chips and small clear crystals below 100 grams in weight, called “lascas” by the trade, are the raw material for fused quartz products. HISTORICAL BACKGROUND The Greeks believed quartz to be permanently frozen water and therefore called it krustallos, which, literally translated, means clear ice; but ages before their civilization, prehistoric man had crudely cut and polished crystals for rough charms and ornaments. About 2000 B.C., the Egyptians brought the art of cutting quartz to a high level. While there are earlier examples of crystal art that have great value, working in crystal during that period became a means of artistic and religious expression that has endured through the ages. Art museums and private collections throughout the world contain many priceless pieces. They include findings from the tombs of the earliest Egyptian rulers, as well as magnificent art objects in both clear and colored crystal encrusted with silver, gold, enamel, and precious gems of oriental and European workmanship. Pierre Curie first measured the piezoelectric effect of quartz, in 188 1, by placing a weight on the surface of a quartz crystal and measuring the resulting electrical charge, which he found was proportional to the weight applied. The following year the inverse piezoelectric effect was proved by the Curies. By applying a voltage to a piece of quartz, a measurable physical displacement occurs. The first practical application of this effect was the construction of a bimorph unit to measure voltage by measuring the amount of the displacement of the end of the bimorph. The piezoelectric properties of quartz crystal remained largely a laboratory curiosity until World War I, when a supersonic device for

Jan 1, 1949

By Hugh H. Waesche

High quality quartz crystals weighing more than 50 grams are required in several important industrial applications.30,31 Primarily, they are the basic raw material for precision, electronic, frequency control components; this includes oscillators and filters in both radio and telephone services. Quartz crystals are also necessary for optical lenses and prisms in special applications requiring high ultraviolet light-transmission as in spectrographs. Quartz wedges are regular components for petrographic microscopes. The application of crystalline quartz as a transducer* in ultrasonic devices has increased in recent years despite strong competition from barium titanate and magnetostrictive [f] devices. Some quartz is fabricated into delay lines for radar. Man has valued quartz for fabrication of art objects since the dawn of history. The art forms were and are painstakingly carved and polished to form intricate figurines, bowls, statuettes, and the well-known crystal balls. The largest known ball, made of perfect quartz from Burma, is now in the National Museum in Washington. It is 12 7/8 in. in diameter and weighs 106 lb 12 oz. Clear, pure quartz chips and small crystals not meeting the electronic-grade dimensional requirements are known by the Brazilian term lasca. They are used to produce fused quartz having wide application in laboratory equipment, as special glasses, for torsion suspension in scientific instruments, and as a source material for growing large artificial quartz crystals 18,35 Electronic applications far exceed all other uses in importance so any discussion of high-quality quartz crystals must be concerned almost exclusively with those functions. Historical Background Because of their ubiquitous character and natural beauty, quartz crystals have long been of interest and known to man. They have been found among early Egyptian and Chinese art forms and the Sumerians are believed to have fashioned seals, beads, and other jewelry from quartz crystals, perhaps 5,000 years ago. Also, American Indians made arrow heads and fashioned some simple objects of different kinds. The origin of the name quartz, although of Greek derivation, is uncertain. The Greeks appropriately applied their word for frozen water or ice, krustallos, to quartz. The present-day, large-scale practical applications of quartz crystals began in 1880-1881 when Pierre and Jacques Curie reported discovery of the "piezoelectric" effect. They found this effect first in Rochelle salt, a common product of grape-wine refineries, while studying crystal symmetry. Piezoelectricity is that property found in certain crystals, including quartz, whereby electrical charges of equal and opposite sign appear on opposite parts of the crystals when they are stressed. If equal and opposite forces are applied to two opposing prism edges of a single untwinned quartz crystal a positive electrical charge will appear on one edge and a negative charge on the other. The amount of the charges will be directly proportional to the force applied. This property seems to be intimately related to pyroelectricity

Jan 1, 1960

By Robert B. McCormick

WORLD WAR II has developed a use for the nonmetal mineral quartz crystal that was unknown in World War I. During the interim period of peace, experimental work in the radio field with the piezoelectric properties of quartz crystal resulted in the almost universal adoption of quartz-crystal radio oscillator plates to control frequency in radio broadcasting, police, commercial and amateur communications equipment. Telephone resonators and filters made from quartz crystal also were developed, which vastly improved the frequency control of long distance telephone circuits. EXPANSION OF THE INDUSTRY The sudden war demands of the armed services for radio equipment using quartz crystal for frequency control led to an unprecedented expansion of the manufacturing industry. It is estimated that the 1940 peacetime volume amounted to approximately $1,500,000, while today a vast new quartz-crystal industry supplies more than $150,000,000 worth of quartz oscillator plates to the Army and Navy each year. This demand has caused an enormous expansion not only of American manufacturing facilities but also of Brazilian mining output, virtually our only source of raw quartz crystal. Actual figures of imports and consumption cannot be cited, for security reasons, but certain comparisons have been made, which indicate the transformation of quartz crystal from a minor to a major nonmetal. Lends has shown that the value of quartz-crystal exports from Brazil is now about equal to that of phosphate rock produced domestically in 1941 and actually exceeds the combined value of crude feldspar, gypsum and fluorspar production in the United States in the same year. This great expansion under wartime pressure was not accomplished without some anxious moments, but all the demands of industry have been met and the Government has been able also to accumulate a substantial stock pile of material against future contingencies. INSPECTION AND GRADING OF QUARTZ CRYSTAL The swift growth of the quartz-oscillator industry necessitated the simultaneous evolution of methods and criteria for inspecting and grading quartz crystal. It has been found that, generally speaking, it is economically feasible to cut only crystals that are at least 30 per cent by volume free from major defects such as optical and electrical twinning, cracks and fractures. Blue needles, bubbles, "chuva" and other minor imperfections can be tolerated in the usable portion unless present in great excess. The present marketing system in use in both Brazil and the United States, as far as quality is concerned, depends solely on the "usability" of a crystal, which is defined in the Brazilian-American agreement2

Jan 1, 1945

By A. M. Gaudin, D. W. Fuerstenau

IN concentration of certain ores by soap flotation, prevention of quartz flotation is desired; the contrary is true in treatment of some oxide iron ores. Experimental study of the flotation of quartz goes back at least a quarter of a century.' Clean quartz does not float with fatty acids or soaps but does float when activated by one of many metallic salts. Control of pH is important. Broadly speaking the problem of quartz flotation has been approached from the empirical side, as was the related topic of flocculation or dispersion of quartz suspensions.' Empirical studies indicated the existence of critical relationships between the additions of collector and activator. These additions were not stoichiometric for the formation of soaps of the activator cation.

Jan 1, 1955