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By H. A. McKinstry, F. F. Lange

A vector analysis of orientating single crystals using the Laue back-reflection X-ray technique is given. Briefly, the analysis involves using a few data taken from a Laue photography and defining the crystal co- ordinate axes in a reference coordinate system. After a few matrix multiplications, the proper goniometer angles can then be determined to orient the crystal coincident with the reference frame. This analysis is easily programed for a digital computer to provide a fast, precise, and efficient method of orienting many crystals which are identical. The general procedure is as follows. The crystal is mounted on a goniometer. Laue photographs are taken until an array of diffraction spots is observed that includes a Laue spot that represents a rotational axis of symmetry. The rotation angles of goniometer are recorded. These angles are defined as positive for a counterclockwise rotation. When the axis of symmetry is located on the Laue photograph, the crystal coordinate axes can be defined in the reference coordinate system* as follows. Two Laue spots are chosen, one of which corresponds to the rotational axis of symmetry and the other to a set of planes whose zone axis is a known crystallographic direction and normal to the rotation axis of symmetry. The Laue spots are used to determine these two crystal directions in the reference coordinate frame. This is done by placing the Laue photograph on a sheet of polar coordinate graph paper and determining the polar coordinates (r, o) of these two diffraction spots in the reference coordinate frame. Their third coordinate is the distance between the crystal and the film (-D). The coordinates Xni of the two crystal directions Nn, (n = 1, 2) in the reference frame are then calculated by the following equations: Xn1 = -D X2n = Ancos on X3n = A, sin on where -tan- 1 rn/D An =Dtan(tan-1rp/D/2) By taking the proper cross products of these two directions (normalized to unit vectors), the crystal coordinate axes 3 (i = 1, 2, 3) can be determined in the reference frame. This is illustrated in Fig. 1. The next step is to determine the relation between

Jan 1, 1969

By C. McDermid

At the request of Mr. C. McDermid, Secretary of the Institution of Mining and Metallurgy, Salisbury House, London, E. C., England, the following reports of standardization committees are here republished. Mr. McDermid invites members of-the American Institute of Mining Engineers to write him and express their opinion of the various proposals made by the committees. COPY OF THE REPORT OF THE WEIGHTS AND MEASURES STANDARDIZATION COMMITTEE OF THE INSTITUTION OF MINING AND METALLURGY, as adopted by the Central Standardization Committee; Dec. 20, 1906, and submitted to the Council, Jan. 16, 1907.

Mar 1, 1907

By ELLSIVOKTH DAGGETT

THE Berlin gold quartz mine is situated in Nye county, Nevada, on the west flank of the Shoshone range, about 40 miles south and 30 miles west from the town of Austin, the county-seat of Lander county. The distance from Austin is about 60 miles by stage-road. The outcrop of the vein, at the top of the incline-shaft, is situated just at the base of the mountain proper, almost exactly at the intersection of the mountain-side with the gravelly bench that slopes for about three-quarters of a mile to the flatter sage-brush plain, or desert valley, below. The -vein itself consists almost entirely of quartz, with perhaps 2 per cent. of sulphide of iron, copper, lead, zinc and antimony, and perhaps a trace of some of the compounds of tellurium with gold and silver, although none of the latter have been as yet positively identified. The relative proportion, by weight, of silver and gold in the ores, varies in different parts of the vein, from 12 silver for 1 of gold, to 7 silver for 1 of gold. The quartz vein-filling is usually frozen fast to the walls, and is very hard and compact, seldom showing the friable, fissured, or shelly structure often to be found in quartz veins. Comparatively little evidence of relative motion of one wall of the vein upon the other is to be found-a fact indicating that during the formation of the vein, and prior to the extensive movements herein described, little disturbance had taken place. No evidence whatever of metasomatic origin has been observed. On the other hand, occasional occurrences of comby structure, in which the axes of the quartz crystals are at right angles to the plane of the vein, rather indicate deposition from solution in a pre-existing fissure. Spurs, or branches, and small parallel veins, while not en-\

Mar 1, 1907

By P. Chiotti, J. T. Mason

Ther?nal, X-ray, metallographic, and vapor pressure data were obtained to establish the phase diagram and standard free energy, enthalpy, and entropy of formation for the compounds in the Sw-Zn system. Four compounds, SmZn, SmZn2 , SmZn4.s, and SmZn8.5, melt congruently at 960°, 94Z°, 908°, and 940°C, respectively. The cornpounds SlnZns, Sm3Znll, and SnzZn7.3 undergo peritectic decomposition at 855", 870°, and 890C, respectively. Another compound of uncertain stoichiometry, SmZn11, undergoes peritectic decomposition at 760°C. Four entectics were observed with the following compositions in weight percent zinc and eutectic tenzperatures in degrees Centigrade: 12 pct, 680°C; 36 pct, 890°C; 58 pct, 850°C; and 72 pct, 900°C. An allotropic transformation and a composition range were observed for the SmZnz compound. The transfor)nation varies from 905" to 865°C as the zinc content increases from 16.0 to 48.5 wt pct, respectively. The free energy of formation of the compounds at 50PC varies between -15.9 kcal per mole for SmZn to -51.1 kcal per mole for SmZn,.,. Corresponding enthalpies vary between -19.2 to -78.3 kcal per mole. The ther-modynamic properties for the liquid alloys are described by the relations: A search of the literature revealed very little information on the Sm-Zn system. Chao et al.&apos; as well as Iandelli and palenzonai have reported the structure of SmZn to be cubic B2 type and Kuz&apos;ma et al3. have reported the structure of -sm2zn17 to be of the Th2Ni17 type. The purpose of this work was to establish the phase diagram of this system, to determine the zinc vapor pressure over the solid two-phase regions of the SYstem, and to calculate the thermodynamic properties of the compounds. MATERIALS AND EXPERIMENTAL PROCEDURES The metals used in this investigation were Bunker Hill slab zinc 99.99 wt pct pure and Ames Laboratory samarium. Analysis of the samarium by chemical, spectrographic, and vacuum-fusion methods gave the following average impurities in ppm: Nd, <200; Eu, <100; Gd, <100; Y, <50;Ca, 225; Ta, 400; Mg, 10; Cu, ~50; 0, 175; H, 20; and N, 15. The elements Fe, Si, Cr, Ni, Al, and W were not detected. The samarium was received as sponge metal and was kept under argon except when being cut with shears and when being weighed. Tantalum was found to be a suitable container for alloys with zinc contents up to the Sm2Znl, stoichio-metry. At higher zinc contents the grain boundaries of the tantalum containers were penetrated by the alloy and the containers failed during prolonged annealing. About 25 g of massive zinc and samarium sponge were sealed in tantalum crucibles equipped with thermocouple wells. These crucibles were in turn sealed in stainless-steel jackets. All closures were made by arc welding under an argon atmosphere. The samples were equilibrated in an oscillating furnace and in some cases were given various heat treatments in a soaking furnace. After appropriate heat treatment the steel jackets were removed and the alloy subjected to differential thermal analysis. The apparatus was calibrated against pure zinc and pure copper and found to reproduce the accepted melting points within 1°C. Alloys were subsequently subjected to metallographic examination and those of appropriate compositions were used for X-ray diffraction analysis and for zinc vapor pressure determinations. The vapor pressures were determined by the dewpoint method. Both the differential analysis and dewpoint measuring apparatuses have been described in earlier papers.4, 5 All alloy samples were etched with Nital (0.5 to 3 pct nitric acid in alcohol) except the samarium-rich alloys. These more reactive alloys were electro-polished in a 1 to 6 pct HClO4 in methanol solution at -700c at a potential of 50 v. EXPERIMENTAL RESULTS Phase Diagram. The results of thermal analysis are indicated by the points on the phase diagram, Fig. 1. Eight compounds and four eutectics were observed. The composition of the compounds and their melting or peritectic temperatures are given on the phase diagram. The four eutectic compositions in wt pct zinc and eutectic temperatures in % are: 12 pct,- 680°C; 36 pct, 890°C; 58 pct, 850°C; and 72 pct, 900°C. The stoichiometry of the most zinc-rich compound is still uncertain, but is very likely either SmZnll or SmZnlz. However, to simplify the presentation which follows it will be referred to as SmZnll. As shown on the phase diagram the phase regions for some of the samarium-rich alloys have not been unambiguously established. A sample of pure samarium was observed to transform at 924°C and to melt at 1074"C, in good agreement with corresponding val-

Jan 1, 1968

By J. E. Andersen, J. Halpern, C. S. Samis

In the presence of oxygen, galena is oxidized in an aqueous medium containing sodium hydroxide, in accordance with the following reaction: PbS + 2O2 + 3OH ? HPbO2 + SO4 = + H2O A novel method was devised for following this reaction which takes place in an autoclave under oxygen pressure, by measuring the concentration of HPbO2- in the solution with a cathode ray polarograph employing stationary platinum electrodes. Using this procedure a study was made of the kinetics of the reaction, in which the effect of a number of variables, including temperature, oxygen pressure, NaOH concentration, and agitation, on the rate, were determined. The results of this study are described and discussed, in terms of possible mechanisms for the reaction. IT is known that sulphide minerals can be oxidized in aqueous media in the presence of oxygen under pressure. Reactions of this type can be classified in two categories depending upon whether the products of oxidation are insoluble or soluble in the aqueous medium. An example of the first type of reaction is the oxidation of pyrite in alkaline solutions, giving rise to an insoluble iron oxide. The kinetics of this reaction have been investigated and its mechanism established.&apos; It has been applied in the oxidation of iron sulphides present in refractory gold ores to improve the subsequent recovery of gold by cyanida-tion.&apos; The second type of reaction finds application where it is desired to recover the metal by leaching during oxidation. In this case a medium is selected in which the oxidized mineral is soluble. For example, nickel, copper, and cobalt sulphide ores can be treated by oxidation in the presence of a solution of ammonia dissolving the nickel, copper, and cobalt as the metal ammine sulphate salts.:&apos; A similar treatment has also been reported to apply to zinc sulphide ores.&apos; It is known that lead sulphate is soluble in solutions of sodium hydroxide or ammonium acetate. It should therefore be possible to dissolve the lead from galena ores by aqueous oxidation with oxygen under pressure using either of these solutions. The applicability of the ammonium acetate treatment has been investigated and confirmed in a recent study.&apos; The present paper describes the results of a similar study in which the kinetics of the oxidation of galena in sodium hydroxide solutions have been investigated. The object of this investigation was pri- marily to obtain information of a fundamental nature relating to the kinetics and mechanism of this reaction. The use of pulps of comminuted ore in a study of this type is undesirable because of the difficulty in controlling and measuring the surface area. The measurements were therefore made using galena crystals of measured surface area and in this way absolute reaction rates were obtained. The reaction was found to proceed as follows: PbS + 2O2 + 3OH ? HPbO2 + SO4 + H2O [I] The products are sodium plumbite and sodium sulphate salts which dissolve in the aqueous solution. The reaction studies were carried out in an autoclave in which a desired pressure of oxygen was maintained. The reaction was followed by measuring the concentration of lead in the solution with a cathode ray polarograph. The results obtained in this investigation are presented and discussed in the present paper. Experimental Materials: The crystals of galena were obtained from Violamac Mines, Sandon, B. C. The following impurities were indicated by spectrographic analysis carried out by the Provincial Assay Office, Victoria, B. C.: Sn, 0.02 to 0.2 pct; Sb, 0.07 to 0.7; Zn, 0.01 to 0.1; Si, Fe, Mg, As, less than 0.05 pct; Ag, 126 oz per ton, the latter determined by standard fire-assaying procedure. After cutting a specimen measuring approximately 5x7x12 mm, the crystal surfaces were ground parallel to the 100 axes using No. 2 emery, washed with water, and the dimensions were measured with a micrometer. Oxygen gas was of commercial grade and supplied in cylinders by Canadian Liquid Air. Solutions were made up with chemicals of chemically pure grade and distilled water. Equipment: Autoclave: The autoclave used in these studies was constructed of stainless steel and

Jan 1, 1954

By F. W. Archibald

The American Smelting and Refining Co. has standardized its copper converting practice to attain a maximum unit blister production with a minimum of refractory consumption by careful location of the tuyeres and by applying magnetite coatings on the hard-burned magnesite brick linings. THE American Smelting and Refining Co. operates four primary copper smelters in the United States with a total of 17 Peirce-Smith type converters; 15 of them are 13 ft in diameter by 30 ft long, and two are smaller. Some details of operations vary with locale; however, fundamentals of design, operation, and maintenance are common to all plants. All converter shells are l-in. thick except for one new converter with riding rings on the ends which has a shell thickness of 1 1/2 in. More tuyeres can be installed with rings on the ends and hence more air can be used. Welded construction is replacing riveted. Minor shell repairs are made after each campaign. Principal causes of complete shell replacement are warpage and cracking resulting from localized over-heating. A 13x30 ft shell is being replaced after 34 years of operation and a total production of approximately 750,000 tons of blister. Converters are driven by 80 hp DC motors through company-designed worm gear reducers. Rotation is 0.38 rpm which permits the skimmer to spot the converter quite accurately for skimming slag. At three of the plants, protection against unscheduled air or power failures is afforded by the installation of emergency drives, consisting of auxiliary air motors or storage batteries. In order to avoid excessive splash out of the converters, the converter mouths are located as far back on the shells as existing flue facilities will permit. At one plant, the back of the mouth is only 13" to the rear of the vertical center line of the converter,. whereas it is 28" at another plant. Newly-lined mouth areas vary from 36 to 44 sq ft with effective operating areas about 25 pct less. It is important to keep the converter mouths as clean as possible. Dirty mouths create back pressures in the converters and as a consequence the tuyere air volumes are reduced. Mouths are generally cleaned by bumping with an empty ladle. Small mouth-cleaning rams have been used but unless extreme care is exercised the brickwork may be damaged. After considerable experimentation, the plants standardized tuyere elevations at 4 to 4% in. below horizontal center line at the shell with a downward pitch of about 13/16 in. per ft of length. Tuyeres are spaced at 6 in. centers except at the riding rings where there are no tuyeres. With this tuyere location, several of the plants now freeze magnetite slag in the bottoms, fronts, and backs up to the bottom of the tuyeres to control the internal shape of the converter. This has the effect of improving the agitation and mixing so that there is a marked increase in converting speed besides affording protection to the brick lining. Currently, the trend is to increase tuyere diameters from 1% to 2 in. to increase the air flow. At present, all converters are hand-punched but one converter is being equipped with a set of mechanical tuyere punchers. Rods for punching are % in. hexagonal smelter bar upset to ll/s in. and rods for cleaning tuyeres are upset to about 1% in., or larger, depending upon the tuyere diameter. Two of the plants use pneumatic reamers for cleaning the tuyeres between charges to minimize disturbing the coating on the inside of the refractory lining. Most of the puncher&apos;s platforms are pneumatically or hydraulically mounted so that a convenient punching position can be maintained regardless of tuyere position. For normal operations, tuyere air pressures vary from 15 to 13.5 psi, although some cycles such as magnetiting require pressures down to 8 psi. Air requirements vary from an average of 25,000 cfm on the newer installations down to 12,000 cfm on the older ones. Converter hoods are designed to protect the punchers from sparks, splash or hood accretions as well as to prevent the escape of objectionable

Jan 1, 1955

By J. E. Lawver, J. D. Raulerson, Charles C. Cook

The agriculture industry has made great strides during the past decade to increase agriculture yields through increased use of fertilizers. Increased use of fertilizers may prevent, or at least delay, mass starvation due to the alarming increase in world population. Phosphate was added to soil as a plant nutrient in the form of calcined bones at least 2000 years ago (Anon., 1964), and man has used phosphate minerals as a source of fertilization in one form or another for at least 100 years. During 1977 the world produced about 116 Mt of phosphate rock, with about 86% used for fertilizers and another 4% for animal feed supplements. More than three-fourths of the total production comes from the United States, Morocco, and the Soviet Union. From a mineral beneficiation point of view, the major sources of phosphate rock and the methods of beneficiation can be classified as follows: marine deposits not containing appreciable carbonate minerals, marine deposits requiring a francolite carbonate mineral separation, igneous deposits not containing appreciable carbonate minerals, and igneous deposits requiring apatite carbonate mineral separation. [ ] Guano, mostly from Chile and Peru, accounts for 0.1% of the total world production, and the calcium phosphates from Ocean, Nauru, and Christmas Islands and the aluminum and iron phosphates from Brazil and Aruba account for less than 4% of the world production and are thus not considered in this classification (Lawver, et al.). At present, marine phosphorite deposits account for about 75% of the world&apos;s production; the igneous deposits account for 20%. The igneous deposits low in carbonate minerals are easily concentrated by crushing, grinding, and apatite flotation. The most important igneous deposits are those of the Kola Peninsula, USSR (Woodrooffe, 1972). The igneous deposits high in carbonate materials are of corn appreciably more difficult to beneficiate, but they have been concentrated by froth flotation for a number of years. An interesting but rather complicated flowsheet of this type is at Phalabonva, in the Republic of South Africa (Lovell, 1976). The Phalaborwa deposit is an igneous complex of pyroxenite with a central core of carbonatite surrounded by a serpentine- magnetite-apatite rock called phoscorite. The phoscorite containing about 10% P2O5, 35% magnetite, and 35% calcium magnesium carbonate is currently being processed. The process involves comminuting the material for fiberation and subjecting it to a copper float using a potassium amyl xanthate as collector and triethoxybutane as a frother followed by a magnetic separation of the tailings to produce a feed for phosphate flotation. This process produces a phosphate concentrate containing greater than 36% P2O5 at a P2O5 recovery ranging from 75 to 80%. Considerable success has been claimed for recovering apatite from carbonate-bearing ores at the Jacupiranga Mine of Serrana S/A (Silva and Andery, 1972). The carbonatite currently being mined contains an average of only 5% P205 and is concentrated using a unique flotation process (Andery, 1968) to yield 96% P205 concentrates. The ore contains about 12% apatite, 5% magnetite, 80% calcite plus dolomite, and minor amounts of phlogopite, olivine, zircon, ilmenite, and pyrochlore. Feed preparation consists of crushing to -31.75 mm (-1 M in.), rod milling in closed circuit with hydrocyclones to about 92% (-50 mesh), and two-stage cyclone desliming of the -50 mesh sands at 20 m. Weight recovery in the deslimed feed is normally 85 to 88% and the corresponding P2O5 recovery is usually about 90%. The deslimed feed is conditioned at 60 to 70% solids for 15 min at pH = 8-10 with 0.6 kg/t of causticized starch for iron oxide and calcite-dolomite depression. The conditioned slurry is diluted to 20 to 30% solids, about 0.2 kg/t of fatty acid or soap collector is added to the conditioner discharge, and the reagentized ore is subjected to rougher-scavenger flotation with additional fatty acid added to the scavenger float. The scavenger concentrate is returned to rougher circuit distributor, and the rougher concentrate froth is subjected to two stages of cleaner flotation to yield a final apatite concentrate analyzing 36 to 38% P205. Flotation recovery of P205 is, in general, above 90% when treating fresh carbonatite. The high-carbonate flotation tails normally analyze 1 % P2O5 or less and are suitable for portland cement production. The marine deposits. Types 1 and 2 of central Florida are representative of enormous reserves of phosphate rock that will undoubtedly account for much of the world&apos;s production in the near future. Until very recently the sedimentary deposits high in carbonate minerals (Type 2) have not been considered reserves due to the difficulty in making a francolite-carbonate separation. Although no commercial plant has yet been built to beneficiate Type 2 ore, laboratory and pilot plant data indicate the process is viable. If so, the reserves of Florida and similar deposits throughout the world will be substantially increased. A discussion of the beneficiation of these two types of sedimentary deposits and the relation of the resulting concentrates to the fertilizer industry of the United States is the subject of this paper.

Jan 1, 1981

By H. H. Klepfer, M. E. Snyder

UNTIL very recently, the commercial availability of the rare earths as metals has been very limited. Fabrication of mill products from these metals has not been studied in most cases. This note reports the results of the development of fabrication techniques for thulium. Thulium has a melting point of about 1550°C and a hexagonal close-packed crystal structure. It oxidizes in air to give a black oxide (TmzO,). The procedures for producing thin thulium foil were developed on one ingot weighing about 220 g and were subsequently applied in processing about a pound of metal to foil. Several alternates for the various fabrication steps were investigated and will be discussed. The metal fabricated was in the form of commercial chill-cast ingots 1 in. in diam and 2 in. long weighing approximately 220 g. Impurities in the ingots were reported by the vendor to be 4000 ppni tantalum, 2000 ppm calcium, 200 ppm nickel, 100 to 200 ppm iron, 100 ppm europium, and less than 100 ppm copper, lutetium, and ytterbium. In addition to these impurities, several salt-like inclusions as large as l/8 in. in diam were revealed along the center line of the one ingot sectioned. Preliminary tests indicated that small wafers cut from the as-cast ingot would not fabricate readily by rolling. Forging of copper-jacketed wafers was therefore attempted. At 1550"F forging was satisfactory but an apparent reaction of copper with thulium demanded investigation of lower temperatures. Therefore, the remainder of the test ingot was forged at 1450°F—with only minor cracking. All ingots forged were inserted into copper tubes of 1 in. 1D and 0.125-in. wall thickness. The jackets were sealed by flattening the ends of the tubes and welding under helium. Heating time at 1450°F was 30 min. Press forgings of 1/8 in. per pass were used, followed by 10 min reheats. When the ingots had been squared and reduced to 0.250 in. in thickness, the original copper jacket was stripped off and replaced by a new jacket in preparation for hot rolling. Hot rolling at 1450" F without edge cracking was readily accomplished after forging. Excellent results were obtained with 10 pct reductions of thickness followed by 5 to 10 min reheats. After reduction of thickness from 0.250 to 0.100 in. the copper jacket was removed. It was found, in fact, that hot rolling in air was possible. A tenacious black oxide similar to that seen on zirconium was formed during 3 min reheats at 1450°F. Reduction in air to 0.010 in. foil was possible taking 10 pct reductions per pass. The oxide coat formed during hot rolling in air could best be removed by sand blasting and pickling. Common pickling solutions containing polar solvents were found to attack the metal too rapidly and a concentrated nitric-hydrofluoric acid mixture attacked neither the oxide nor the metal. The most satisfactory pickling solution was 52 vol pct concentrated nitric acid-48 vol pct glacial acetic acid. After forging to 0.250 in., vacuum annealing and cold rolling was found to be another satisfactory alternate to hot rolling in copper jackets. After forging. a hardness of Rockwell B76 was found. Annealing in vacuum (2 X l0-5 mm of Hg) for 1 hr at 1200"F did not alter this value. Annealing at 1470"F for 1 hr brought the hardness down to R;]63. With cold rolling (5 pct per pass) the hardness returned to about R,1:76 after 20 pct reduction and edge cracking became noticeable. However, cold rolling to a total of 40 pct reduction in thickness (RI,,83) was possible before edge crack propagation became serious. Good surface finish was obtained, and the metal loss due to oxidation was minimized by cold rolling and vacuum annealing. Using this procedure the yield of 1.25 in. wide by 0.010 in. thick foil from a 1-in. diam ingot was about 40 pct.

Jan 1, 1961

By J. C. Holm

ALTHOUGH the main constituents of Portland cement are the oxides of calcium, silicon, aluminum, and iron, characteristics of the cement are seriously affected by such contaminants in the raw materials as magnesium, phosphorus, sodium, potassium, sulfur, and others of lesser importance. Sources of cement raw materials comprise a long list of minerals occurring in nature in various degrees of purity. The calcareous raw materials are generally limestone of purity varying from calcite to cement rock (a low-grade limestone of natural, almost correct chemical composition), chalk, marl, seashells, coral, and coral sand. The argillaceous raw materials supplying silicon, aluminum, and iron are mainly various forms of clay and shale, to which may be added silicious sand, iron ore, bauxite, or kaolin for minor adjustment of the chemical composition. The quality of Portland cement in this country, as in most parts of the world, is controlled by rigid specifications limiting both its chemical and physical characteristics, and cement manufacturers must comply with these specifications to market their products. Brandon Raw Materials: An unusual deposit of marl, limestone, and clay occurs 12 miles east of Jackson, Miss., near the village of Brandon. The deposit is of sedimentary origin and of relatively young geological age. Layers of marl vary from putty-like consistency to such hardness that it can be cut with a knife. Interspersed between the layers of marl are bands of limestone varying from very soft to hard. the compressive strength of the hardest layers exceeding 15,000 lb per sq in. The layers of marl range in thickness from a few inches to about 25 ft. The limestone bands seldom exceed 2 to 3 ft but often occur in thinner veins in the quarry face. Above the top layer of the deposit, which may be marl or limestone, a layer of clay ranges in thickness from a few inches to more than 20 ft. Part of this clay is harvested with the raw material to supply part of the argillaceous components, but most of it is stripped as overburden and wasted. A highly silicious clay of extreme fineness, harvested from the bottom of the quarry below the marl and limestone bands, is to correct the silica content. Fig. 1 shows typical examples of the interrelation of the various materials, based on drill logs obtained during exploration of the deposit. The marls vary in moisture content in the bank from 15 to 30 pct and contain up to 70 pct -200 mesh particles and up to 40 pct —10 p particles. A large percentage of the fine fraction is within the colloidal range, making the marl extremely sticky. The limestone beds range in hardness from that of the hardest marl to a medium hard limestone and in moisture content from 2 pct to approximately 14 pct. The line of demarcation is often difficult to draw and the moisture content is possibly the best means of classification. The ratio of soft to hard material is not constant throughout the deposit, but the average is approximately 70 pct soft to 30 pct hard material. Through the years this deposit had been repeatedly explored by cement companies and rejected as unsuitable for cement manufacture, mainly because of physical characteristics. In 1950, after careful exploration of the deposit and comprehensive laboratory and pilot plant tests of the raw materials, officials of Marquette Cement Mfg. Co. of Chicago were convinced that a practical and economical method of processing the raw materials had been devised and authorized construction of a new plant that began production in December 1951. Marl and limestone, common raw materials for Portland cement, usually occur in such a manner that they can be worked separately. Their harvesting and processing normally have presented no difficult problems, as standard equipment and methods are available for handling either sticky or hard materials. No other cement plant utilizes a deposit of the nature of that at Brandon, however, and for this reason no prior art was available for design. When properly blended, the raw materials produced an excellent cement without additives. Basic problems to be solved in designing the cement plant were:

Jan 1, 1957

By Joseph C. Mead, Alan Stanley

The MacIntyre Development of the National Lead Co. is located at Tahawus, N. Y. The operations involve the mining and concentrating of a titaniferous iron ore to produce an ilmenite concentrate and a magnetite concentrate. Construction of the MacIntyre plant was commenced during the summer of 1941,when world conditions threatened to cut off the supply of Indian ilmenite. An open pit mining operation was developed and the crushing and milling equipment put in operation in July 1942. A general description of the operation was given in the Adirondack Issue of Mining and Metallurgy for November 1943. The metallurgy of the mill operation was described by Mr. Frank R. Milliken,* Plant Manager, National Lead Company, MacIntyre Development, and presented at the AIME New York Meeting, February 1948. The magnetite concentrate produced in the milling operation was too fine (minus 20 mesh) to be used directly in iron blast furnace operation, and most of the magnetite had to be stockpiled in 1942 and 1943. In 1943, the Defense Plant Corp. built a Greenawalt sintering plant at Tahawus, N. Y., to put the magnetite concentrate in a more suitable form for use in the iron blast furnace. The Greenawalt sintering plant consists of three 10 by 25 ft sintering pans designed to produce 1800 gross tons of sinter per 24 hr. The vacuum to each pan is produced by two Greenawalt fans in series, pulling approximately 30,000 cu ft of air per minute at 50 in. water gauge vacuum. The plant started operation in August 1944. The present plant production averages 25 tons per operating pan hour (approximately 224 lb per operating hour per square foot of grate area) of plus 1 in. sinter. Raw feed to the plant consists of 61 pct magnetite, 4 pct anthracite coal culm, and 35 pct minus 1 in. return fines which are conveyed to a pug mill where the materials are mixed thoroughly and water added to give the mixture 5.5 to 6 pct moisture. The mixed prepared feed is conveyed to two 4 by 10 ft vibrating screens where the minus 1 in. plus 5/8 in. return fines are screened out and discharged into a surge bin for use as a hearth layer. The minus 5/8 in. prepared feed is discharged into another surge bin for use as prepared feed. A charge car, electrically operated, having a capacity of one charge of prepared feed and several charges of hearth layer, lays a thin layer of plus 5/8 in. return fines and 9½ in. depth of prepared feed into the pans. A fluffing roll and a vibrator on the car fluffs and spreads the prepared feed into the pans. An ignition car, electrically operated, ignites the top of the bed with a 30 sec flash burn. The 9½ in. bed sin-ters in approximately 13 min. Dumping the pan, and recharging and igniting the bed requires 2 min. To improve the quality of the ilmenite concentrate produced in the mill and to reduce the amount of titanium dioxide lost in the mill tailings and in the magnetite product, extensive research work and pilot plant operations have been done on grinding the crude ore to minus 65 mesh size (rather than to minus 20 mesh) and concentrating it by a combination of magnetic separation (for magnetite recovery) and flotation (for ilmenite re-covery). These tests have proved successful in increasing ilmenite re-covery and grade. With the development of the ilmenite flotation process to a stage where a full scale flotation plant was in the design stage, the problem arose of handling the 65 mesh magnetite concentrate that would be produced. In order to study and solve the problems of handling and sintering the 65 mesh magnetite in the sinter plant, a pilot sinter plant was secured from John E. Greenawalt. The effect of using 65 mesh magnetite in the sintering operations was then studied on the 2.4 sq ft test pan, operating under conditions as similar to the large plant as could be set up in the laboratory. A series of tests were run in the test pan on present sinter plant feed that had been mixed in the plant pug mill. An average production and an average quality of sinter produced in this series

Jan 1, 1950

By T. S. Lundy, R. A. Padgett

The fact that cobalt diffuses in silver at a much slower rate in a region near a free surface than in bulk material has been demonstrated in a variety of experiments. Various possible mechanisms of this near-surface effect (NSE) are examined in light of experimental evidences. The tendency for surface segregation of some solute atoms appears to be a likely mechanism to explain the effect. UNIDIRECTIONAL and isothermal diffusion from a plane source of radioactive tracer into an isotropic, homogeneous medium follows the Gaussian solution to Fick&apos;s second law, or: where A(x,t) is the position and time-dependent concentration of the diffusing species, M is the quantity of diffusant per unit area initially at x = 0, and D is the diffusion coefficient. For a given time, say t = tl, one can easily see that: d In Aixji)_____1_ r2] d(x2) 4Dti Thus, if diffusion data obtained by serial sectioning are plotted as In A(x,tl) vs x2, the diffusion coefficient is obtained from Eq. [2]. The ideal behavior seldom is observed in real systems. Deviations from ideality generally occur either at small or large values of penetration distance. The overall picture is shown schematically in Fig. 1 where Regions I, 11, and 111 are due, respectively, to some near-surface effect or effects (NSE), volume diffusion, and short-circuiting effects. For different systems and conditions of specimen preparation and analysis, the relative importance of Regions I, 11, and I11 may be drastically different. Region I is completely absent in many systems and there is no NSE. In others, however, there may be considerable difficulty in determination of volume diffusion coefficients due to the overshadowing influences of Region I. Such is particularly true when indirect techniques such as the surface concentration decrease or the Gruzin method&apos; are used to find D. In this paper several experiments which had as their goal a better understanding of near-surface effects are reported. Specifically, it is well-known that unusual penetration behavior results for the diffusion of several impurities in ilver- and that considerable controversy exists with regard to interpretation of the published diffusion data. We chose to examine those unusual results which occur for cobalt diffusion in monocrystalline silver395 primarily because knowledge of experimental procedures and materials were readily available. Both radioactive co60 and co5&apos; could be utilized to offer a wide range of available concentration of the diffusing species. Experiments were also performed on the diffusion of AgnO in silver. They gave base-line data for the system—both for technique evaluation and for examination of the vacancy distribution near the surface. I) PROCEDURES Cylindrical-shaped specimens 1.25 cm diam and 1 to 1.25 cm long were cut from 99.999 pct Ag single crystals obtained from Monocrystals Co., Cleveland. One end surface of each specimen was polished flat and etched with a mixture of 20 ml saturated Cr03 solu-tion-20 ml H20-3 ml concentrated HC1. Radioactive tracer (co60 or co5&apos; or Ag&apos;lO, each having a radio-chemical purity of greater than 99 pct) was deposited onto the prepared surface either dropwise with evaporation to dryness of the solution containing the tracer (0.5 N HC1 solution for the co60 and co5&apos; and 0.6 N HNO3 solution for the A"&apos;), by electroplating, or by evaporation from a tantalum or tungsten filament in an evacuated bell jar. The amount of deposited cobalt was varied from many atomic layers of cobalt containing the co60 to approximately one co5&apos; atom per lo6 surface atoms of silver. This large variation in amount of deposited cobalt yielded information about both the influence of a thick-source layer of tracer and solubility effects on the NSE. Such variations were possible because of the large differences in half-lives,

Jan 1, 1969

By C. H. Ault, D. D. Carr

Four counties in Indiana- LaPorte, Vigo, Vanderburgh, and Switzerland-have potential for deep underground limestone mining because they are in or near high population areas and have no surface-mineable limestone deposits. The principal markets are Gary-South Bend, Terre Haute, Evansville, and Cincinnati. Mineable seams suitable for aggregate are 120-150 m (400-500 ft) below the surface in LaPorte and Vigo Counties, about 90 m (300 ft) below the surface in Switzerland County, and about 600 m (2,000 ft) below the surface in Vanderburgh County. Some deposits are also suitable for high-purity uses or for cement raw materials, which enhances their potential for exploitation.

Jan 1, 1983

By J. J. Gilvarry, B. H. Bergstorm

The first part of this paper describes a new approach to the problem of energy relationships in fracture and comminution. The basic theoretical method used (as contrasted to previous empirical or semi-empirical approaches) is an attempt to verify or disprove the hypothesis of von Rittinger, In the second part of the paper, theoretical conclusions for the three headings of single fracture, plural fracture, and comminution are tested. Agreement between theory and experimental results is demonstrated. The classical hypotheses on the energy relationship in brittle fracture are those of von Rittinger-that the energy required is proportional to the new surface formed— and the alternative one of Kick.&apos; Over the years, repeated attempts have been made to discriminate experimentally between the two assumptions, or to replace both of them, as has been done by Bond? However, no semblance of agreement seems to exist among different investigators. This paper is the first in a series essaying a new approach to the entire problem of energy relationships in fracture and comminution. The purpose of this program of research is to verify (or disprove) the hypothesis of von Rittinger. In contrast to previous empirical or semi-empirical approaches to the problem, the basic method adopted is theoretical. The prime aim is to determine the distribution function for fragment size theoretically and to verify the predicted distribution experimentally. This approach should make possible determination of the total surface of the particles by integration over the corresponding distribution function; one may hope that this direct procedure will yield more definitive results than use of gas adsorption or other methods. The surface area so obtained can then be compared with experimental energies, as obtained by Bergstrom, Sollenberger, and Mitchell,4 for example. It is convenient to distinguish between single fratture, plural fracture, and comminution. Single fracture of a brittle solid is defined as fracture by an external stress system which is removed instantly and permanently when fracture is initiated. Plural fracture consists of single fracture of the original specimen, followed by a sequence of only a few secondary fractures; comminution differs in that the sequence of secondary fractures consists of a large number of repetitive steps. For single fracture, Gilvarrys has given a rigorous derivation of the proper distribution function for fragment size, based on a closely defined physical model and deduced strictly by the laws of probability. Gilvarry and Bergstrome have compared the predictions of the theory with experiment, and have found excellent agreement. The prior work of Gilvarry and of Gilvarry and Bergstrom considers only single and plural fracture. The purpose of the present paper is to extend the discussion to the case of comminution. For prefatory purposes, the theory of Gilvarry for single fracture will be outlined. The considerations will then be applied to the cases of plural fracture and comminution. SINGLE FRACTURE The derivation is based on the Poisson law.7 For Points distributed with mean density y over a domain, this law states that the probability p(t)dt of one point lying in the range t to t + dt with none in the interval 0 to Ms p(t)dt = ye-yt dt. For this distribution to be valid, it is necessary and sufficient that the points be distributed at random, individually and collectively in the sense of ~~~.7 The former qualification requires that the position of One Point be independent of another, and the latter implies that the probability of a region containing a

Jan 1, 1961

By C. G. Dunn

This note describes a method for revealing micro-structures in tantalum through an {hkl} effect which was found during a study involving amorphous and crystalline tantalum oxides. Three steps are involved. First, an amorphous film of Ta2O5 is formed anodically1 on the surfaces of the tantalum. The amount needed depents on the thickness of the substrate tantalum; 1600Å of oxide, however, is generally satisfactory in the 1/2 -mil (12 µ) to 3-mil thickness range. The film at this point is uniform in color. Second, the anodized specimen is heated to 800°C in. vacuo during a period of a few minutes and held at temperature for 5 min. During such a treatment some oxygen leaves the oxide through dissolution into the substrate tantalum (e.g., at 10-8 Torr oxide films thinner than about 800 completely disappear on 5-mil strip). Considerable crystallization of the amorphous oxide also occurs adjacent to the metal/oxide interface but not throughout the oxide thickness. The thickness of oxide needed as a residue is not too critical; values between 500 and 1000Å (optical estimate&apos;) may be most useful. (The presence of a residual oxide layer after the heat treatment usually is not apparent; in fact, in most instances the surfaces have a metallic appearance. This can be the case also for thicker residual films needed in the detection of a crystalline oxide phase by surface X-ray diffraction—e.g., if the initial oxide film is 3000Å thick, enough crystalline oxide is formed for X-ray detection.) The third step eliminates the metallic appearance at the surface and reveals (or produces) a varied colored film of tantalum oxide. Two methods can be used and both will be illustrated. If the specimen is dipped in 48 pct HF for a few seconds, the tantalum is found to be covered with a multicolored oxide. Moreover the colors correlate with the grain structure of the substrate tantalum through an orientation dependence of the type illustrated in Fig. 1, where results of an orientation analysis by the Laue X-ray method have been plotted. Other film conditions would have provided a different set of colors for the same orientations. Any such correlation, however, provides a basis for a qualitative assessment of the distribution of orientations in a large sample. The cold-rolled structure of tantalum foil produced by a recrystallization anneal and a cold-rolling reduction of 95 pct is not easily obtained by usual metal-lographic methods.&apos; The structure, however, is easily revealed by the present technique, Fig. 2. The alternative third step is to reanodize the specimen. The optical nature of the final anodic film depends on the presence of the crystalline oxide phase; color variations indicate optical thickness variations in the film. As the reanodization voltage is increased from zero, straw and light brown colors appear (as usual), followed now by variations in color from grain to grain depending on {hkl} orientation. Suitable end points, which are determined by voltage and time, are easily established. Fig. 3, for example, shows the grain structure developed in 5-mil tantalum strip during a 30-min re-crystallization and grap-growth anneal at 1800°C. An anodic film of 1600Å thickness was added prior to the special 800°C anneal. Reanodization was done at constant current density (near 0.2 ma per sq cm) in an aqueous solution of H3PO4 (0.01 pct) and was terminated after the initial brown colors were replaced by a deep blue at approximately 30 v. Although good grain contrast can be obtained with bright field illumination, even greater contrast for black and white micrographs may be obtained with polarized light, as in Fig. 3.

Jan 1, 1967

By C. W. Price, G. A. Wheeler

BERYLLIUM has always been a difficult material to prepare for metallographic examination. Severe surface deformation occurs during mechanical grinding and polishing, and a suitable bright-field etchant has not been developed. Certain electrolytic techniques produce satisfactory polishes, but these techniques have not yielded entirely consistent results. Furthermore, they have not provided satisfactory bright-field etches. The purpose of this paper is to describe an electrolytic polishing technique that can also provide an excellent bright-field etch. In addition to the bright-field etch, other advantages of this technique are excellent reproducibility, rapidity, and ease of polishing and etching. Experimental Technique. Specimen Preparation. Beryllium specimens may be either mounted or unmounted for the use of this technique, and the size of the specimens is not important. Specimens with surface areas up to 4 sq cm have been electrolytically polished and etched successfully with this technique. The most important requirement is to provide a good electrical contact to the specimens, preferably on the back of the specimens. When specimens are mounted, a hole is drilled through the back of the mount so that the specimen can be contacted with a probe. Conventional metallographic grinding techniques are used to prepare the specimens for electrolytic polishing. The specimens are ground on silicon carbide papers. Grinding through the usual series of papers down to the 600-grit paper is recommended to minimize the electropolishing time, although successful electrolytic polishes and etches have been obtained by grinding only through the coarser papers. A continuous flow of water is used during grinding to provide lubrication and to minimize contamination. Mechanical polishing is not required because high rates of material removal are achieved with the electrolytic polishing. Polishing. Most of the results reported in this paper were obtained with a "Disa-Electropol", manufactured by Struers Scientific Instruments of Copenhagen, Denmark. Satisfactory results have also been obtained with the conventional beaker technique of electrolytic polishing, however, the conditions applicable to both the Disa unit and the beaker technique will be described. Stainless-steel cathodes are used in both techniques. In the beaker technique, a flat cathode, with an area at least twice that of the specimen, is used, and the specimen is held parallel to the cathode. The distance between the specimen and the cathode affects the quality of the electropolish. This distance is set at about 7 mm in the Disa unit; the same distance produces the best results in the beaker technique. Specimen-cathode distances greater than about 20 mm produce considerable relief, while distances less than 7 mm cause high current densities that are difficult to control. An electrolyte of 2 pct HC1, 2 pct HNO3, and 2 pct HCIOl in ethylene glycol gives the most satisfactory results for both electrolytic polishing and etching. This electrolyte was developed by altering the composition of a similar electrolyte used for electrolytic lapping1 and adding HClOl to improve the etching characteristics of the electrolyte. Variations of from 0.25 pct to as much as 5 pct of each of the acids do not significantly affect the results, but the greatest amount of control and reproducibility can be obtained with the composition of 2 pct of each acid. Generally, lesser amounts of the acids produce lower polishing and etching rates, while greater amounts of acids cause high current densities that are difficult to control.

Jan 1, 1968

By John E. Conley

The production of lime by the burning or calcination of limestone, including all varieties from true dolomites and magnesian limestones to high-calcium types, continues as one of the essential basic industries. In 1937, a total of 4,124,165 tons of lime valued at approximately $30,091,000 was produced in the United States.&apos; The importance of any contribution to our knowledge on the mechanism of the lime-burning process is, therefore, obvious. The burning of limestone has been practiced since the earliest days of our civilization, and the literature on the various phases of the industry is voluminous. Calcination of the various types of limestone has been studied by many previous investigators, but some points require additional research. Each occurrence of limestone provides an opportunity for specific investigation, because the characteristics of stones in different localities vary. Knibbs13 has given an excellent discussion of available data on the theory of lime and magnesia burning. The thermal dissociation of calcium carbonate has been studied more recently by Johnstonr2 Smyth and Adams,3 Ralston et al.,4 Furnas,6 Potapenko,6 and Southard and Royster.7 As a result of these investigations the dissociation temperature at atmospheric pressure has been established as 894" to 898&apos; C. The dissociation of dolomite and magnesite, although studied by several investigators,4,6,8 still requires clarification by additional data. The calcination of limestone was studied for a twofold purpose: (I) to extend our information on the mechanism of the lime-burning process and (2) to standardize the conditions for calcination of high-calcium and dolomitic limestones for subsequent hydration tests on the lime.

Jan 1, 1942

By John E. Conley

The production of lime by the burning or calcination of limestone, including all varieties from true dolomites and magnesian limestones to high-calcium types, continues as one of the essential basic industries. In 1937, a total of 4,124,165 tons of lime valued at approximately $30,091,000 was produced in the United States.&apos; The importance of any contribution to our knowledge on the mechanism of the lime-burning process is, therefore, obvious. The burning of limestone has been practiced since the earliest days of our civilization, and the literature on the various phases of the industry is voluminous. Calcination of the various types of limestone has been studied by many previous investigators, but some points require additional research. Each occurrence of limestone provides an opportunity for specific investigation, because the characteristics of stones in different localities vary. Knibbs13 has given an excellent discussion of available data on the theory of lime and magnesia burning. The thermal dissociation of calcium carbonate has been studied more recently by Johnstonr2 Smyth and Adams,3 Ralston et al.,4 Furnas,6 Potapenko,6 and Southard and Royster.7 As a result of these investigations the dissociation temperature at atmospheric pressure has been established as 894" to 898&apos; C. The dissociation of dolomite and magnesite, although studied by several investigators,4,6,8 still requires clarification by additional data. The calcination of limestone was studied for a twofold purpose: (I) to extend our information on the mechanism of the lime-burning process and (2) to standardize the conditions for calcination of high-calcium and dolomitic limestones for subsequent hydration tests on the lime.

Jan 1, 1942

By K. B. Nowels

DATA pertaining to pipe line flow for both oil and gas in horizontal or nearly horizontal pipe lines are both extensive and accurate. However, the pipe formulas used to determine pressure drop for flowing fluids (liquids and gases) under conditions of horizontal flow are not generally applicable to flowing oil and/or gas wells. Except for some data developed in small laboratory set-ups, little or no information was available concerning flow of oil and gas mixtures in vertical pipes, when, in 1928, the writer began the development of a method for computing pressure drops in the pipes of flowing oil wells, as outlined in this paper. In 1929, Uren1 presented some findings based on laboratory experi-ments in which vertical flow of an extremely heavy crude oil was induced, by means of air through a 2-in. pipe, 41 ft. long. The friction factors derived from the experiment, as well as values for pressure drop per 100 ft., are not believed satisfactory in their application to flow problems in the field. Versluys,2 also in 1929, presented a mathematical development of the theory of flowing oil wells, and in 1930, gave a companion paper3 setting forth some principles governing the choice of length and diameter of tubing in oil wells. Since the termination of the study presented in this paper, another. valuable contribution pertaining to the problem, of vertical flow was made by Moore and Wilde.4 Although there were writings dealing with the principles of the gas-lift, a search of the available literature indicated that specific information on vertical flow was lacking with the exception of the writings of Uren, Versluys, and Moore and Wilde, to which reference .has been made.

Jan 1, 1932

By Robert Williams

A description is given of a double heat treatment of 60-40 brass. Photomicrographs are included to show the changes that take place in the microstructure on reheating the water-quenched specimens. A wide variation in the mechanical properties may be obtained by the described heat-treatment method. ON SEVERAL occasions, when 60-40 brass is first obtained in the beta condition by quenching at about 825° C. and is then reheated, the writers have noticed that recrystallization will take place in the form of twin crystals at the grain boundaries of the original beta crystals. It was, therefore, thought that interesting results would be obtained if this twinning process was studied further, especially as to the temperature at which it first occurs. The material used in the investigation was a bar of extruded muntz metal, 1/2 in. in diameter, and of the following composition: Copper, 60.21 per cent.; zinc, 39.73 per cent.; lead, trace; iron, trace; tin, nil. Specimens I in. in length were sawed from this bar and a hole was drilled into the side of each specimen until it reached the center, and the tip of a platinum-platinum rhodium thermocouple was inserted. A small Hoskins&apos; resistance-type electric furnace was used for heating the specimens. The specimens were first heated at 840°C. for 2 hr. and then quenched in cold water, in order to get the material entirely in the beta state. In every case, in the reheating process, the furnace was brought to the desired temperature before the specimen was introduced. The time occupied in preheating was from 20 to 30 min. By sawing back 1/4 in. on each side of the hole, two parts were obtained from each specimen

Jan 3, 1924

By B. N. Thompson

Main industrial minerals produced in New Zealand are nonmetallic - clay, dolomite, limestone, pumice, salt, serpentine, and silica sand. Other minerals, some with minor production, include diatomite, feldspar, magnesite, sulfur, asbestos, and perlite. Energy and metallic minerals and aggregate are excluded from this account. These industrial minerals occur in a wide range of rock types and geological ages. For example, clays are known from the weathering products of Cretaceous rhyolite and leaching of Eocene coal measures; from Quaternary weathering of contemporary loess and shallow marine sediments, and of greywacke of Triassic-Jurassic age; and from the hydrothermal alteration of late Cenozoic acidic volcanic rocks.

Jan 1, 1984