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My bets are on you, every time! But who is right? In the "cobalt issue" of our favorite magazine, January 1951, you stated: "By far the best immediate United States prospect for, large amounts of cobalt is the Blackbird mine of the Calera Mining Co., which is operating for Howe Sound Co., in Leinhi County, Idaho." In the March 1 issue of Saturday Evening Post, Ernest F. Mechlin, Jr., chief cobalt section, National Production Authority, states: "The Bethlehem Steel Co.'s Cornwall, Pa. ore bed is the principal domestic source." Maybe he should have said: "was the principal domestic source", or perhaps Howe Sound's Idaho cobalt is still in the prospect stage in Mr. Mechlin's opinion, perhaps in yours too. KATHARINE W. CARMAN GEOLOGIST 933 MICHIGAN AVE. EVANSTON, ILLINOIS Mr. Mechlin is correct in his statement that Cornwall is the principal domestic source of cobalt, but within the year, Blackbird production should greatly exceed that from Cornwall. Calera is expected to ultimately produce 3 million lb per year, whereas Cornwall averages 520,000 lb per year. -Editor.

Jan 1, 1952

By Rupert Spivey

Kennecott Copper's Chino mine is one of the oldest copper mines in the United States, having been operated by the Spaniards as early as 1800. At that time haulage methods were indeed primitive. Indians brought the ore up on "chicken ladders" in leather buckets. It was then melted into crude bars and hauled to Chihuahua by mule train. There are still remnants of the old trails near the present pit where the mule hooves cut grooves in solid rock. The mines were worked as underground operations off' and on until open-pit mining was started in 1910 by John Sully and Daniel C. Jackling. Since that time many haulage methods have been used: mule carts, steam and electric trains and finally large haulage trucks, now believed to be the best method for this mine. The general shape of the pit is oval with dimensions of 1% miles by 1% miles. Working benches are 50 ft high, with the bottom bench at 5750 ft and the top at 6450 ft above sea level.

Jan 1, 1964

By Francis Flynn

MANY excellent papers, descriptive of the milling and smelting of every kind of commercial ores, the refining of virgin metals, the casting into various shapes demanded by the trade, the rolling into shapes best suited to the factory machinery and the making of composition alloys to suit every requirement have been issued by the many technical societies dealing with non-ferrous metals. It is a wonderful collection of papers, of which the mining and metallurgical engineers may well be proud, but strange as it may seem, metallurgists in general appear to take the stand that when they have delivered suitable alloys to the foundry and rolled products to the factory their duty to write papers has ceased, at least in so far as the A. I. M. E. is concerned. Still we read in the daily papers that the mining companies are absorbing metal-manufacturing industries. The purpose of this paper is to describe the reclaiming of non-ferrous scrap metals at manufacturing plants, taking as an example the automobile industry.

Jan 1, 1929

[A AALSETH, EARL P GEOLOGIST. AMERADA PETROLEUM CORP. BOX 1498 BILLINGS. MONT ABADIE, HENRY G ASST TO SUP OF OPER LONG BEACH OIL DEVEL. CO. 255 S. SANTA CLARA. LONG BEACH, CALIF. ABBE. TRUMAN W. … ASST.FLD.SUP.OF PROD SUN OIL COMPANY BOX 66 STOWELL. TEXAS ABBOTT. J. L. .... GEOL. PARTNER PRITCHARD & ABBOTT 504 CENTURY BLDG. FORT WORTH, TEX ABBOTT, RICHARD H OWNER ABBOTT AND HOWARD OIL 422 W. HERMOSA DR. SAN ANTONIO, TEXAS. ABBOTT, SETH J.. JR PETR ENGR.]

Jan 1, 1961

By J. J. Gilman

THEORIES of fracture in metals have been based primarily on the dependence of fracture strength on grain size. This dependence was first observed by Masing and Polanyi.l These workers, as well as 0rowan12 and Davidenkov and Wittman,' thought the grain size could be equated with the crack size in the Griffith condition for crack propagation.4 In this way they could account for the observed proportionality between fracture stress and the reciprocal square root of the grain size. The chief results of recent investigations of the fracture strength of polycrystals are summarized in Fig. 1. Low for iron,5 Petch for iron,' Greenwood and Quarrel for zinc, Petch and Zein for zinc,' and Hauser, Landon, and Dorn for magnesium'' have all found that the fracture stress of a polycrystal is proportional to the reciprocal square root of the grain size. Also, they find that, for large grain sizes, the fracture stress lies near the extrapolation of the yield-stress curve determined at small grain sizes; where measurable plastic strain precedes fracture. Low9 has gone a step further and shown that, in Range 1, the fracture stress in tension is almost identical to the yield stress in compression for a given grain size. Homes and Gouzou, 10 and Low also have shown that, in Range 2 of Fig. 1, microcracks form when the yield stress is reached, but they do not cause failure until the stress reaches a much higher value. The fact that yielding always precedes fracture suggests that fracture is induced by plastic flow. A mechanism by which this might occur was first proposed by Zener.11 He pointed out that blocked dislocations would cause stress concentrations which might cause fracture. The blocking would be caused by grain boundaries. This idea has been developed by Eshelby, Frank, and Nabarro,12 by Koehler,13 and by Stroh.14 By means of etchpits blocked dislocations have been observed in brass by Jacquet,15 in zinc by Gilman,16 and in lithium fluoride by Gilman and johnston. The blocked-dislocation theory and the experiments that bear on it have been summarized by Mott.18 One of the strong points of the blocked-dislocation theory is that it can explain the grain-size dependence of the fracture stress in a natural way. However, Low9 has pointed out that the theory is not satisfying when it is considered quantitatively. Gilman10 also has criticized the theory and presented an alternative interpretation of the relation between fracture stress and grain size. Since the blocked-dislocation theory is not the only theory that can explain in the grain-size effect, it is necessary to find other evidence either to support or deny it. In this investigation the following points were studied: 1) If blocked dislocations normally cause fracture, then the fracture stress ought to be very high in the absence of plastic glide. Is it? 2) If dislocations must be blocked in order for metals to fracture, then certain types of grain

Jan 1, 1959

[Abrahamson, Guy C., (5'43) Lt., 0-880861, Hammer Field Fresno Calif. Adamec, LAW, (8'42) c/o Braden Copper Co., Rancagua, Chile. Adams, Karl S., (9'43) Univ. of New Hampshire, Durham, N. H. Agnilar, Roperto Q., (9'43) Texas College of Mines, El Paso Texas. Ainge, B'onald Farra, (943) Otago University, Dunedin, New Zealand. Akaran, Cevdet A,, (9'44) Pennsylvania State College, State College, Pa. Albala, Americo, (5'44) School of Mineral Industries, The Pennsylvania State College, State College, PA.]

Jan 1, 1946

By K. Osseo-Asare

LIX63 In combination with DNNS selectively extracts nickel and/or cobalt from acidic leach liquors with pH values as low as 10 Nickel/cobalt and cobalt/nickel selectivities are achieved by varying the relative concentrations of LIX 63 and DNNS Increasing LIX63 concentration retards both extraction and stripping rates while DNNS has the opposite effect. Slope analyses of equilibrium data Indicate that both LIX63 and DNNS are present in the extracted complexes. Examples of possible flowsheets are presented.

Jan 1, 1981

BOSTON SECTION ALFRED C. LANE, Chairman, GEORGE A. PACKARD, Vice-chairman, H. M. BOYLSTON, Secretary-Treasurer, R. L. AGASSIZ, FRED W. DENTON. The forty-ninth meeting of the Boston Section was held at the Boston City Club on Monday evening, Dec. 23, 1918. The meeting was preceded by an informal dinner at which 29 members and guests were present; three or four others came in later. The reading of the minutes of the previous meeting was dispensed with by consent.

Jan 2, 1919

By AIME AIME

THE session on milling methods on Monday afternoon.* with G. H. Clevenger, chairman of the Mining Methods Committee presiding, was well attended. However, none of the authors of the papers presented were present except Messrs. Taggart and Ince. The paper on "Elements of Operations of the Pneu¬matic Table," by Messrs. Taggart and. Lechmere-Oertel, was presented by Professor Taggart as was the paper on "Calculations in Ore Dressing," by Luyken and Bierbrauer, due to the absence of the authors.

Jan 1, 1929

United Engineering Trustees, Inc James L Head, '55, E C Meagher, '56, Gail F Moul¬ton, '57 Advisory Committee to Real Estate Committee Cleveland Dodge, Herbert Hoover, Paul D Merica The Engineering Foundation W M Peirce, '56, A M Gaudin, '58 Research Procedure Committee A M Gaudin, March '54 Engineering Societies Library Board Frank T Sisco, '54, E M Wise, '56, James L Head, ex officio Engineering Societies Personnel Service Board of Directors E J Kennedy, Jr, E H Robie

Jan 1, 1954

EXECUTIVE COMMITTEES OF LOCAL SECTIONS Arizona E. P. MATHEWSON, Chairman W. V. DECAMP, First Vice-chairman F. W. MACLENNAN, Second Vice-chairman E. D. GARDNER, Secretary-Treasurer, U. S. Bureau Of Mines, Tucson, Ariz. MICHAEL CURLEY J. P. HODGSON HENRY F.1 ASTER CLYDE E. WEED Boston Meets first Monday each winter month GEORGE A. PACKARD, Chairman FRANKLIN B. RICHARDS, Vice-chairman F. LEROY FOSTER, Secretary-Treasurer Rooms 8-219 Mass. Inst. of Tech., Cambridge, Mass. G. W. METCALFE D. H. MCLAUGHLIN

Jan 1, 1932

By Renato G. Bautista, KNona C. Liddell

A model of the reaction of chalcopyrite, CuFeS2, with Fe3+ and with 02 is considered. Homogeneous solution phase reactions are assumed to be always at equilibrium throughout the dissolution of the mineral. The dissociation of USOb- and several complexation reactions involving cu2+, Fez+ and Fe3+ are incorporated in the model equations. The relative importance of Fe3+, 02, and H+ as oxidants and the role of solution equilibria are assessed and the implications for leaching practice discussed.

Jan 1, 1981

[Alphabetic Section: The letter immediately following a member's name indicates grade: M-member, A-associate, J-junior. The numerals following member's grade indicate year of election. The letter following year of election indicates primary divisional affiliation: A. Mining & Exploration F. Coal B. Minerals Beneficiation G. Petroleum C. Iron and Steel H. Industrial Minerals D. Extractive Metallurgy J. Council of Education E. Institute of Metals K. Council of Economics Geographic Section: An asterisk (*) preceding a member's name indicates availability for consulting work:]

Jan 1, 1961

DR FRANK DAWSON ADAMS Montreal, Canada HENRY STURGIS DRINKER Bethlehem, Pa PROF HATON DE LA GOUPILLIERE Paris, France SIR ROBERT A. HADFEILD London, England HERBERT C. HOOVER Leoben, Austria ROBERT W. HUNT Chicago, ILL JAMES FURMAN KEMP New York, N.Y. PROF HENRI LOUIS LE CHATELIER Paris France EZEQUIEL ORDONEZ Mexico City, Mexico ALEXANDRE, POURCEL Paris, France RICHARD H, RICHARDS Boston Mass. JOHN E. STEAD Middlesborugh, England PROF DIMITRY CONSTANTIN TSCHERNOFF St Petersburg, Russia CHARLES D WALCOT Washington D.C.

Jan 1, 1923

By J. B. Newkirk, A. H. Geisler

The alloy Cu4Pd has a disordered face-centered-cubic structure when quenched from temperatures between 478ºC and the melting point (about 1100°C). Below 478ºC an ordered phase is stable. The results of a Debye-Scherrer X-ray analysis indicate that the ordered phase has a tetragonal unit cell described by the space group C24h — P42/mt with 2 Cu in 2a, 2 Cu in 2f, 4 Cu in 4j (x = 0.2, y = 0.6), 4Pd in 4j (x = 0.4, y = 0.2), and 8 Cu in 8k (x = 0.1, y = 0.3). The orientation relationship between the face-centered-cubic phase and the ordered tetragonal phase is given by: [100],,. // [130]al,. COO1Ia.d.//COO1I,,.. • The behavior of Cu,Pd is typical of ordering alloys except that the transformation is very sluggish. The increase in hardness and the microstructural and X-ray diffraction effects are interpreted in terms of coherency strains caused by the ordering. AN anomalous construction in the Cu-Pd phase diagram (Fig. 1) was reported in 1939 and has been allowed to stand without further published attention since that time. The odd figuration about the composition 10 to 27 atomic pct Pd is derived mostly from the work of Jones and Sykes.1 Evidently several features of this binary system require further study if the constitutional forms are to be well understood. The present paper includes a study of one of these features, that is, the crystal structure of a single ordered alloy containing nominally 20 atomic pct Pd. This choice of composition was suggested by the work of Harker and associates who determined the structure of Ni4Mo2 and Ni4W.3 The nature of the ordering process in Cu4Pd was studied also by observing the hardness, microstructure, and Debye-Scherrer patterns of specimens which had been aged at various temperatures after quenching from an initial disordering treatment. Experimental Methods A 20 gram ingot of Cu4Pd was made by melting spectrographically standardized copper from Johnson, Matthey, and Co., and commercially pure (99.5 + ) palladium in an argon-filled quartz tube. Chemical analysis showed that the ingot contained 80.0 atomic pct Cu. The ingot was rolled about 60 pct to a strip 0.060 in. thick and was homogenized for 16 hr at 950°C in low pressure argon. Rods cut from the rolled strip were worked into wire 0.015 in. in diameter, and specimens for hardness and microscopic examination were cut from the remaining strip. All specimens, with the exception of some of the wire, were given an initial disordering treatment by heating for 16 hr at 950°C, followed by water quenching. A 10 cm length of as-drawn wire was water quenched after being held in a temperature-gradient furnace4 for 89 days. Room-temperature Debye-Scherrer photograms were then made at points along the wire to determine the temperature below which the ordered phase was stable. Although the accuracy of temperature determination in the gradient was only about ±10 °C, the temperature gradient was sufficiently gradual that the sensitivity was much better and locations which had differed by as little as 1°C could be distinguished. An analysis of the crystal structure of the well ordered alloy was made by X-ray diffraction using a specimen cut from this wire. The change of Debye-Scherrer pattern as ordering progressed was studied by using isothermally aged samples of initially disordered wires. The wires were sealed under low-pressure argon in small quartz tubes for heat treatment. After the aging treatment, the tubes were quenched in water and photograms were made at room temperature in a 10 cm diam camera using filtered Cu kX. (A = 1.540511) Hardness was measured on a Vickers hardness tester using a 10 kg load and 2/3 in. objective lens. Reported values are the average of at least three impressions made on flat specimens 0.060 in. thick. After the hardness of a heat-treated sample had been measured, it was resealed in low-pressure argon and returned to the furnace for continued aging at the same temperature. In this way, two samples served for all aging times at each temperature. Hardness specimens which had been aged 500 hr or more were used for metallographic examination after the final aging treatment. A dilute potassium-dichromate etching solution was used.

Jan 1, 1955

By O. W. Simmons, L. W. Eastwood, C. M. Craighead

H. Schwartzbart and W. F. Brown, Jr.—The authors have divided the effects of recovery on the true stress-true strain curve into two types; metarecovery, which effects only the first part of the curve or the yield strength, and orthorecovery, which effects the flow stress at any strain. Both of these are said to be true recovery effects, involve no recrystallization, and are explained by the removal of two different types of imperfections caused by work hardening. However, there seems to be some question as to whether the data are sufficiently conclusive to exclude, as an explanation of the authors' results, a mechanism based on the relief of residual stresses between the grains or slip bands and recrystallization. It appears that metarecovery could be interpreted in the same fashion as a customary interpretation of the Bausch-inger effect. The balanced system of internal stresses which exists between grains in a strained specimen due to varying orientation and, hence, yield strengths, of the different grains is responsible for a reduced yield strength in compression following pre-tension, and, similarly, for an elevated yield strength in tension following pre-tension. If the specimen is now heated so that the internal stresses are relieved by creep, then the yield strength in tension following tension will have been reduced and in compression following tension will have been raised. There seems to be a very strong case for the lack of recrystallization in the aluminum investigated by the authors, if one defines recrystallization as the presence of visually detectable new grains or accepts the X-ray evidence as conclusive. One must remember, however, that the appearance of spots on the back-reflection X-ray patterns cannot be taken as the time when recrystallization first started. The areas of recrystallized strain-free material must first have grown to a size large enough to give distinct spots on the patterns and this may take some time. Averbachl7 in an investigation of brass has shown that recrystallization can be detected by extinction measurements at temperatures lower than those based on hardness or X-ray line width determinations. It can be seen from fig. 10 that the rate of recrystallization is extremely low over a considerable time period at the onset of the process. Observations on the rate at which small amounts of recrystallization effect the flow stress would have given further insight as to whether undetectably small amounts of recrystallization might have been responsible for orthorecovery. Also, the question arises as to whether the effects observed in fig. 6 for various times and temperatures could not have been obtained if the time at 212°F were sufficiently long. In addition, the argument that the curve in fig. 10 is not sigmoidal seems weak in view of the scattering of the points. It is conceivable that an accurate determination of the curve for the first 100 hr would exhibit a relationship other than the one drawn. There is one point we would like to raise about the condition of the starting material. The authors annealed their material at 750°F for 15 min to remove the effects of any previous work hardening or machining strains. Reference to the work by Anderson and Mehl shows that this treatment may not have completely recrystallized the aluminum, so that the starting material may have had some strained areas. Higher temperatures or longer times may have been required to remove the effects of any small strains. We would like to mention some results of tests being conducted at the Lewis laboratory of the National Advisory Committee for Aeronautics in an investigation of the Bauschinger effect in relation to fatigue. Tests were performed on annealed electrolytic copper and several annealed brasses. Specimens were pre-strained 1 pct in tension and then tested in compression or tension with and without intermediate stress-relieving annealing treatments at 500°F for various times. Specimens heated at 500°F for 10 1/2 hr showed an elevation of the flow curve in compression and an approximately equal lowering of the flow curve in tension when compared with the curves for the un-heat treated specimens. After approximately 0.8 pct strain, all flow stresses coincided and were equal to the flow stress of the virgin material at this strain. This behavior is consistent with the metarecovery observed for aluminum by the authors and for which a residual stress model can be used. On the other hand, increas-

Jan 1, 1951

By J. H. Collier

The mother lode, or mineralized belt, at Angels, in Calaveras county, California, is 3 miles wide. At least, a region of that width has been, and is being, prospected which has shown considerable mineralization. The lode proper divides into three lodes, or groups of veins, at this point. On all of these branches, mines have been operated with more or less success.

Jan 1, 1900

By Frank T. Weems

The basic operating properties of the DorrClone are discussed and certain metallurgical applications which exploit these properties are presented. An effective method of controlling the consistency of the DorrClone underflow is described. THIS paper presents in a general manner some of the applications of the DorrClone (Dutch States Mines cyclone) in the metallurgical and heavy chemical fields. Technical or mathematical analyses of the design factors and of the mechanism whereby the cyclone effects its separation have been capably treated in a series of previous papers.'-' Engineering and operational aspects of a few installations and laboratory tests have been chosen to emphasize the unique classification characteristics of the DorrClone and to illustrate its utility in certain difficult situations. Its use in coal washing and heavy-media operations are not considered. Some 25 or more industrial installations and applications of the DorrClone in the metallurgical fields are operating at present, ranging from single trial units to complete batteries composed of a multiplicity of units. The data were obtained in part from some of these, and in part from operations of units at the Westport Mill, the laboratories and testing plant of the Dorr Co. at Westport, Conn. The DorrClone was developed, in principle, by the research dept. of the State Mines, Limburg, Holland, during World War 11. Its first use was to dewater a —50 micron sand used as a dense medium in coal washing. The metallurgical wet cyclone was first publicized by Driessen and Yancey and Geer.6 ince then the cyclone has been studied as a means of de-watering, heavy media concentration, and fine size classification. The DorrClone is shown in Figs. 1 and 2. pulp to be treated is pumped through the feed nozzle, A, into the feed cylinder, B. The feed nozzle is of rectangular cross-section, the outermost edge being tangent to the feed cylinder walls. Feed shims, C, may be attached to the innermost walls to adjust the open area of the feed nozzle available to entering pulp. The tangential injection of feed under pressure supports the vortex action of the pulp that has been detained in the cyclone; the centrifugal forces of this vortex throw the coarse particles to the walls of the cone, D, where they collect and pass downward and out through the adjustable apex opening, E. The fine particles contained in most of the water that entered with the feed pulp move to the inner spiral of the vortex and flow out through the vortex finder, F, contained in the orifice plate, G, which forms the top of cyclone chamber. The overflow pulp may then spray freely into a spray chamber, H, surmounting the cyclone or pass directly into a 90' elbow, I, of somewhat larger diameter than the vortex finder. Installation Where more than one cyclone is to be installed, best overall efficiency and ease of control are obtained with equal distribution of both pulp volume and weight of solids among the cyclones, and with the same pressure being maintained at each cyclone feed nozzle. Fig. 3 is a suggested arrangement for feeding two or more cyclones in parallel. Feed pressure control: Under normal operating conditions it is not unusual for some surge to exist in the feed that is to be sent to the cyclone. As will be discussed later, surges in the solids content of the pulp are usually not of great operational consequence, but surges in feed volume are a problem. Several systems have been devised for absorbing surges in feed volume, each involving a surge tank. If the surges are small and fairly rhythmical, a tank of sufficient size might be installed to dampen out

Jan 1, 1952

By J. B. Wagstaff, R. A. Buchanan, J. F. Elliott

High speed photography through blast-furnace tuyeres showed coke particles moving rapidly. Model studies showed a raceway was formed and gave quantitative results which were correlated with actual blast furnaces. Another study showed the similarity between hanging and the flooding of a packed column. This was explored by models. THE combustion zone before the tuyere in an iron blast furnace is a vital region because here are generated: 1—most of the gases on which the furnace depends to carry out its basic operation of reducing iron ore to the metallic state, and 2—the major fraction of the heat required in the nearby regions of the furnace for the various reduction reactions, the fusion of the slag, and the melting of the iron. Since the greater part of the coke is consumed in this region, the descent of the burden must be greatly affected by the characteristics of the tuyere zone. This region then would seem to be a profitable field for study. Fortunately, a view into this important zone is available to the operator through the tuyere peep sight. Here he sees relatively dark pieces of coke "dancing" in the blast. What he sees is of considerable help in interpreting the behavior of the furnace at a given time but the very rapidly moving particles and the intense radiation obscures what is happening very deep in the zone. This investigation was initiated in the hope that a better understanding of the combustion region could be obtained by using a high speed camera with a maximum speed of 3000 frames per sec. It seemed the best practical method of "slowing down" this characteristically violent action within the highly luminous field. Model studies and tuyere probing also have been used to aid in explaining the observed phenomena. Above the combustion zone, but below the fusion zone, there is probably a region in which the coke is comparatively stationary. Here are zones in which the gases must flow up through the granular bed counter to descending liquid slag and metal. There is no easy way to observe this zone in a blast furnace, but model studies have been of some help in explaining the nature of the zone and the laws governing the flow of the fluids involved. The whole problem is difficult and involved and any approach to a complete solution may require long investigation. This preliminary report has been written, therefore, because it is believed that appreciable progress has already been made that would be of interest to others. Tuyere Studies, Chemistry and Kinetics It is well known from the early work of Kinney and coworkers1,2 that combustion of carbon before the tuyeres appears to occur in two zones: Zone A: C + O, = CO2; AH77°F. = — 14,108 Btu per lb of carbon [I] Zone B: CO2 + C = 2CO; H77°F = + 6,183 Btu per lb of carbon [2] Zone A (Fig. 1) is close to the tip of the tuyere and zone B is somewhat farther back; there being a transition region in which both reactions occur. It is interesting to estimate the rate at which coke is burned before a tuyere with a wind rate of 90,000 cfm in a modern furnace having 18 tuyeres. Approximately 0.55 lb of carbon is consumed by eq 1 per tuyere per sec. A like amount disappears by eq 2 for a total consumption of 1.11 Ib per sec per tuyere. Assuming the coke is 85 pct C and has a bulk density of 30 lb per cu ft, this figure can be converted to a total of 1.30 lb of coke with a bulk volume of 0.043 cu ft disappearing per sec per tuyere. At the temperatures prevailing in the combustion zone (according to Kozlovich,³ he maximum is about 3400°F), the rate at which carbon is con-

Jan 1, 1953

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

PST 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. The X-ray diffraction analysis of chemical compounds of crystalline form has proved of inestimable value for structure studies and rapid qualitative analytical purposes in a number of fields.' In some cases X-ray diffraction analysis has been found suitable for quantitative determinations. H. P. Klug2 found that quantitative procedures for quartz powders when mixed with calcium fluoride were reproducible within ±1.0 pct. Talvenheimo and White3 reported quantitative analyses of clay minerals to be accurate within 10 pct and also detected 1 pct of bentonite in 99 pct illite. In other investigations,'" powders of quartz and mica have been analyzed quantitatively with accuracies from 1 to 5 pct. A powder of tungsten carbide was analyzed similarly by Redmond7 and Rooksby8 reported the determination of small amounts (0.11 pct) of calcium oxide in magnesium oxide. In the most generally practiced use of X-ray diffraction, traces of the diffracted beam are recorded as lines on a film much as lines of elements are recorded on an optical spectrograph film. As with the spectrograph, the darkness of the lines denotes the amount of the constituent in the sample. If the film is replaced by a Geiger tube assembly and a graphic recorder or a scaling unit, the intensity of the diffracted beam can be registered as a peak on a chart or energy impulses per unit of time on the scaler. Several methods of quantitative measurement have been investigated and reported in literature. Klug2 used manual operation of the goniometer and a counting technique to determine the difference in counting rates at the diffracted angle and for the background. In another case3 the area under the recorded diffracted peak was the basis for the determination. In other instances the height of the recorded diffraction peak above background, measured while the goniometer was moving, has been the basis for the measurement. The sizes of particles most suitable for diffraction techniques are reported in the literature as follows: for tungsten carbide a maximum of 40 microns7 and for quartz a maximum of 5 microns.' Very fine sizes of crystals are known to cause a broadening of the diffused beams; hence some workers have set a lower limit of 0.1 micron for quantitative results. Guinier10 has indicated that broadening of the diffracted X-ray beam is not appreciable for crystallites larger than 0.02 to 0.03

Jan 1, 1956