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By Arthur Hockman, Howard W. Jaffe, Howard F. Carl

THE problem of establishing practical techniques for evaluating natural corundum ores arose from the desire to improve the existing purchase specifications for crystal corundum procured by the Federal Government for stockpiling. Such purchase specifications had been developed for a large number of products, including minerals and ores considered to be critical and strategic because of the country's dependence on foreign sources of supply. It will be apparent to anyone considering the subject of purchase specifications that the determination of whether or not a submittal meets the specifications is a prime consideration. Consequently satisfactory specifications for minerals should not only incorporate physical, chemical, and mineralogical requirements that are practical but should also establish the means by which both buyer and seller can be assured that materials meet stated requirements. The Munition Board's Material Purchase Specification for corundum, dated February 1954, covered two grades of crystal corundum intended primarily for abrasive use. It established limits of size and of composition: Grade A, at least 95 pct +3 mesh and 92 pct alumina (Al2O3); Grade B, at least 95 pct +7 mesh and 90 pct alumina. It also specified that "of each lot of material, not less than 95 percent shall have a hardness equal to or exceeding nine (9) on Moh's Scale." These specifications were unsatisfactory for several reasons. They did not allow the purchase of lower grades of corundum being used by industry. Neither did they specify exactly what a corundum ore actually was, except that it should contain so much alumina and have a certain scratch hardness. Nothing was said about the abrasive qualities of the material that was to be purchased primarily for abrasive use. During the period 1946 to 1948 supplies of the two grades defined in the then current specifications continued to decrease. Early in 1949 industry recommended that the finer sizes of corundum known as "crystal corundum concentrates," ¼-in. to 16-mesh material, be added to the stockpile specifications and that lower grades of crystal corundum also be included. In the spring of 1949 the National Bureau of Standards and the Bureau of Mines were asked by the Munitions Board to cooperate in developing more practical specifications for grading natural corundum ores. The National Bureau of Standards indicated that it would investigate physical test methods for determining abrasive characteristics of corundum, and the Eastern Experiment Station of the Bureau of Mines at College Park, Md., stated that it would consider the mineralogical aspects of the problem. Members of these two agencies, in consultation with representatives of the Office of Materials Resources of the Munitions Board and of the Federal Supply Service of the General Services Administration, and with the cooperation of industrial suppliers and consumers of abrasive corundum, developed, in a fairly short time, more practical specifications for six grades of corundum ores. The new specifications, issued January 1951, were for corundum, natural crystals, as by this time high-purity synthetic corundum was available and widely used. Nevertheless, for certain specific applications the natural product was preferred over the synthetic material. It has been extensively used in forming snagging wheels. It breaks into more or less cubical particles, whereas artificial corundum fractures into splintery shapes. These produce irregular cuts in glass, while the more symmetrical shape produces a more uniform ground surface. For this reason natural corundum has been preferred for certain types of lens grinding. Pure corundum is clear, colorless alpha alumina (A12O3), but it is rarely found in nature in this form. The most important gem varieties include the blue and yellow sapphires and the ruby. Minute impurities of titanic oxide impart a blue color,

Jan 1, 1955

By M. T. Hepworth, W. B. Sample

HYDROGEN solubility and linear contraction measurements were made at constant temperature on an alloy of titanium of constant oxygen-to-titanium molal ratio but variable hydrogen content. A cylindrical specimen of titanium (0.25 by 1.6 in.) containing 0.75 at. pct 0 and less than 0.03 at. pct N was cast from a master button of iodide process titanium which had been alloyed with titanium dioxide. Four vacuum fusion analyses, which were made along the length of the cylinder after the hydrogen solubility studies were made, revealed a variation of oxygen content of less than 0.02 at. pct. The specimen was introduced into a quartz furnace tube, annealed and outgassedat 1050"~ for about 1 hr, and then held at 800" * 0.5" for about 30 hr, during which latter time experimental data were taken. The leak rate to the furnace chamber was not sufficient to contaminate the specimen during the run as determined by leak-rate studies and vacuum fusion analyses for oxygen and nitrogen before and after the runs. The furnace chamber was attached to a modified Sieverts apparatus used to introduce measured quantities of purified hydrogen to the specimen. A quartz pushrod transmitted changes in length of the specimen to a Chevenard dilatometer. The push-rod passed through a vacuum grease seal to the dilatometer which amplified motion of the rod by a factor of 319. During hydrogen addition, the pushrod did not contact the specimen. Measured quantities of hydrogen were added to the specimen and equilibrium hydrogen pressures recorded as a function of hydrogen content. The solubility data, which appear in Fig. 1, agree well with a separate investigation made with a different apparatus. The solubility limit of the hcp a phase appears as an abrupt discontinuity in slope at 3.4 at. pct H. The solubility plot has been extended as a dashed line at this discontinuity in order to emphasize the discontinuity. The hydrogen content at which bcc P appears is not clearly defined. An arrow indicates solubility data were taken upon hydrogen addition. Upon reaching the arbitrary maximum hydrogen content of the run, the quartz pushrod was pressed against the specimen in order to record the change in length with hydrogen removal. A pressure of about 100 g per sq cm was required to overcome the friction of the vacuum seal in order to obtain reproducible linear contraction data. The contraction ratio ~2/1", change in length divided by original length, was set equal to zero for the maximum hydrogen content. The relative contraction of the specimen was observed upon removal of hydrogen in the following manner. The system was opened to the pumps for a few seconds and an unknown quantity of hydrogen was removed. The system was then isolated from the pumps by closing a stopcock and allowed to return to equilibrium. When the temperature returned to 800°C, the pressure stabilized, and contraction ceased, measurements of contraction and pressure were made. The hydrogen content of the specimen was then deduced by measuring the equilibrium PIydrogen pressure and referring to the solubility plot. Linear contraction was then plotted against interpolated values of atomic percent hydrogen. The justification for this procedure is the established reversibility of the hydrogen equilibrium.' Uniaxial compression was assumed to have no effect on hydrogen pressure. The isothermal linear contraction data are plotted on Fig. 1. An arrow indicates data were taken upon removal of hydrogen. The solubility limits of the two phase a i /3 region can be identified by discontinuities ill slope of the dilatometric plot at 9.1 and 3.4 at. pct H, agreeing well with other studies.' Dashed extensions of the plots emphasize the discontinuities. Isothermal studies of expansion made upon hydrogen addition gave curves of much smaller slope and less pronounced discontinuities. A uniaxial compressive stress tends to accentuate volume changes in going from the more open bcc phase to the hcp phase.2 Incomplete data on ex-

Jan 1, 1962

By C. G. Dunn

The measurement of interfacial teusions or grain boundary energies in metals is an important metallurgical problem, especially since it bears on growth and nucleation processes. Statistical methods of measuring equilibrium grain boundary angles, which relate interfacial tensions, have been used by some investigators1'2 but more direct methods would be preferred. A direct way, based on a simple extension of a successful method of growing single crystals of silicon ferrite to predetermined orientations in flat specimens,3 is to produce three-grain specimens in such a way that the equilibrium common grain boundary will be perpendicular to the surface of the specimen. The angles to be measured then appear as the grain boundary angles in the surface of the specimen. The method of producing a single crystal specimen with a predetermined orientation is basically the same as that employed by Yoshida and Fuji-wara4 in their work on aluminum wires. The specimen, prior to any single crystal transformation, must have a matrix which will support the growth of a crystal of the desired orientation. Growth may occur through exaggerated grain growth or, if the matrix is strained a critical amount. by normal recrystallization. In either case the matrix must have stability at the temperature used to effect the transformation, this stability appearing as a long induction period for exaggerated grain growth or for the formation of recrystallization nuclei. Additional control is gained by using a high temperature gradient through which the specimen is moved at a suitable rate. To obtain the desired orientation, the specimen is fed a short way into the furnace producing one or more crystals in the hot end. After the specimen is removed from the furnace, the orientation of a crystal is determined, so that this crystal may be reoriented by properly deforming a narrow piece of the matrix between the end crystal and the rest of the specimen. This part of the specimen in the case of silicon ferrite is preferably held at red heat during the reorienting process. Fig 1 shows a specimen which is ready to be transformed into a single crystal through growth of a reoriented "seed" crystal. When the method just described is applied to the production of a three-grain specimen two crystals are grown first side by side in one end, the specimen is then reversed and the third grain grown from the opposite end. A suitable group of grains each of different orientation is one where all three grains have the same crystallo-graphic plane in the plane of the specimen. Fig 2 shows a photograph of a three-grain group prepared as described. The notches are introduced in the open ends of the grain boundaries to anchor them during the final annealing operations which ultimately should bring the grain boundaries to the lowest energy configuration. Two-grain groups with different crystallographic planes in the plane of the specimen can be similarly prepared and treated. If the two grains have different surface (gas to metal) energies per unit area, the equilibrium condition leads to a curved grain boundary.* * This feature of the problem was pointed out by J. c. Fisher. References 1. Cyril Stanley Smith: Grains. Phases and Interfaces: An Interpretation of Microstructure. Trans. AIME 175, 15. Met. Tech. TP 2387, June 1948. 2. D. Harker and E. Parker: Grain Shape and Grain Growth. Trans. A.S.M. (194,5) 34, 156-195. 3. C. G. Dunn, A. Seddon, and R. Wylie: Unpublished Work, 1946-1947. 4. Takeo Fujiwara: A Method of Producing A Long Single-Crystal Wire of Aluminum with any Desired Crystallographic Axis. Jnl. of Sci. Horoshima Univ. A, (1939) 9, No. 3, 227.

Jan 1, 1950

By C. Gatlin, C. E. Nemir

A common cure of lost circulation is the introduction of granular bridging agents into the mud system. Many materials, such as ground nut shells, are used for this purpose. If the trouble causing void (fracture, fissure, vug, etc.) is not too large, the granular agent forms a "bridge" across or within the opening. Successively smaller particles in the mud stream then accumulate on and/or within this bridge until normal filtration is finally established. The efficiency of many bridging agents has been studied in the laboratory using various slot testers.',' Many investigators have remarked that a granular bridging material should have the proper particle size distribution. With the exception of the broad range specified in the patent of Goins and Nash,3 here is apparently no definition as to what this distribution should be. A bridge may be initiated when several particles of lost circulation material lodge against each other in a fracture or other void. Smaller particles then may bridge the openings between the larger, previously bridged particles. This process continues until the voids become quite small and the problem becomes one of filtration. It would seem logical that an optimum particle size distribution exists, i.e., one containing the proper quantity of properly sized material to fill the successively smaller voids of the bridge. The filtration characteristics of drilling fluids may be subject to a similar analysis. It has been clearly demonstrated by many workers that the filtration behavior of various muds can be altered by particle size control.'.' Slusser, et al, divided filtration into three periods and showed that particle sizes affecting a given period did not necessarily affect other portions of the filtration curve. An analagous problem is the proper sizing of gravel, liner slots and screen sizes in various sand-exclusion problems. Here the situation is reversed in that a proper "void" size, rather than the size of the bridging agent, is sought. The classic work of Coberly 9 forms the quantitative basis for most sand-exclusion processes. It is interesting to note that, in general, Coberly's work has been overlooked by most drilling-mud researchers. Other investigators have made various studies of the effect of particle size distribution .on drilling-mud properties. As a part of their studies, Fancher and Oliphant reported 30-minute filtration loss of a variety of mixtures of particle sizes.'' Gates and Bowie noted an effect of particle size distribution on filtration, as well as on other physical properties.' MAXIMUM DENSITY THEORY A maximum density mixture has been mentioned as the possible solution for both lost circulation and mud filtration problems. Furnas 12 derived mathematically a method for obtaining maximum density of beds of packed solids, having either a given number of component sizes or a continuous gradation of sizes. This work was verified experimentally by Anderegg.13 or mixtures having a continuous grading of sizes, the interval between sizes is taken as successive screen sizes of interval 2 The ratio of the quantity of each size and the next smaller size is given by the equation Fig. I, number of size intervals of ratio 2 taken from Furnas' paper, gives the value of n + 1 for any given values of + and K, where K is the ratio of the diameter of the smallest particles to the diameter of the largest particles. Measurement by weight assumes, of course, constant density for all particle sizes. Choosing the quantity of the smallest particle size as a unit weight, the required weights of the successively larger interials are then r1 r2 r3 . ®1,2,3. Thus, the grading curve of a maximum density mixture represents a geometric pro gression of ratio r.

By S. F. Reiter, R. W. Guard, J. H. Keeler

DURING the last several years the authors have been conducting tests on a tensile machine that autographically records load-elongation data. In certain tests at elevated temperatures on face-centered cubic, hexagonal close-packed, and body-centered cubic materials (binary alloys of nickel, zirconium, and iron), the load-elongation curve as shown in Fig. 1 reaches a maximum load (Pmax,) at relatively small amounts of strain and a large amount of elongation occurs subsequently with a continuously decreasing load, until finally localized necking and fracture take place. This early maximum load behavior has been found without the accompanying evidence of localized necking as has been assumed by some, or of evidence of cracking as observed by others.' This behavior has also been observed by Nadai and Manjoinez whose results are in good agreement with ours. The prior strain, strain rate, test temperature, and crystal structure affect the observations. The influence of prior strain was observed in tests on unalloyed zirconium at 300°C in which specimens containing large amounts of prior strain (cold work) exhibited the type of curve shown in Fig. 1. No localized necking was observed after strain as much as that of point B. Annealed and recrystallized specimens of the same material showed a load-elongation curve with maximum load occurring after considerable strain hardening and at the beginning of localized necking. Interrupted tests (Fig. 2) show no loss in strength because of recovery or recrys-tallization during an interval at temperature without load. Recovery under stress such as found by Wood and Suiter3 in aluminum is now being investigated as one possible explanation. The strain rate is a contributing variable as shown in Fig. 3, a test on high purity nickel. Here the strain rate was decreased by a factor of ten during a test in which the maximum load was reached at a small strain. The slope of the true stress-true strain curve was positive with the more rapid strain rate and negative with the slower strain rate. In many binary ferrites an added effect of temperature has been observed. Fig. 4 shows the load-elongation plots for a binary ferritic alloy containing 2 pct Mo. The slope of the small portion of the stress-strain curve obtained at a strain rate of 0.01 mhr1 changes sign from negative to positive on going

Jan 1, 1955

By V 7. 0 / 300 dpi

WHEN the copper smelters were built, in Montana, all of the refractory products which were used in their construction were shipped in from Eastern factories. It was apparent that if a material suitable for the manufacture of these products could be found within the State, a saving of freight could be effected and a new industry built up. Prospecting for such materials was started and experiments were made with samples from numerous deposits. Considerable effort and funds were expended in an attempt to manufacture silica brick from Dillon quartz, a light colored sandstone that is found near Dillon, Mont., on the Oregon Shortline railroad. As a brick material the Dillon quartz was a failure, but it has proved very satisfactory as a silica cement. It is now being used in laying silica brick and for reverberatory furnace bottoms. A bed of quartzite that is particularly suited to the manufacture of high-grade silica brick -was finally discovered at Browns Spur, 6 miles west of Anaconda. The material from this deposit is now being used in the manufacture of the Anaconda silica brick, which have gained a wide reputation for heat-resisting and lasting qualities. The analysis of all average sample of this quartz is: SiO2,, 96.7; Fe203, 0.3; Al203, 2.5; CaO, 0.3 per cent. The very low percentage of fluxing ingredients makes this a most refractory material. All of the Anaconda silica brick are hand molded. Various types of brick machines have been tried, but the hand-mold process proved the best suited to the manufacture of silica brick from this material. The silica is first put through a jaw crusher and is then clumped into wet pans, where 4 per cent. of lime paste is added, to produce a bond. Without the lime the. material would not be plastic enough to mold. After a few minutes' grinding in the wet pans the material is conveyed to the molder, who forces it into the molds by hand. The brick are then dumped on pallets and placed in the drier, where they are left until dry enough to be set in the kilns. Some of the brick are re-pressed before being dried. They are burned about five days, in round down-draft kilns. It is not necessary to have as much heat in the kilns as the brick will be subjected

Jan 9, 1913

By Stephen H. Stow

A relationship exists between the color and the chemical composition of the pebbles from the Bone Valley Phosphate Formation. Darker-colored pebbles are relatively high in iron oxide and relatively low in calcium phosphate when compared to lighter-colored samples; the brown color of the phosphate pebbles can be correlated with their iron content and the black and gray colors with their organic carbon content.1,3 It was anticipated that the darkness of a phosphate sample might be quantitatively measured by a simple reflectivity test and that the amount of reflected light could be correlated with the chemical composition of the rock, especially with the elements which cause the color and darkness of the Florida phosphates. Twenty-one samples of production grade phosphate rock from Hillsboro County, Fla., were studied. All samples were ground to -200 mesh for reflectivity tests and analyses. All analyses are accurate to well within ±2% of the reported value, except for aluminum and organic carbon, which are accurate to only ±15% of the reported amount. Reflectivity measurements were taken with a model 610 Photovoltmeter for tri-stimulus amber, blue and green, and white lights. Experimental procedures and data are available upon request. Results Table 1 contains linear correlation coefficients (LCC) for the element-reflectance relationships for the samples. The top portion of the table refers to the LCC between the percent of light reflected off the samples and the percent of a given element (or its oxide) as analyzed. In the lower portion of the table the LCC refers to the relationship between the same reflectance data and the chemical analyses which have been corrected on the basis of 0% acid insoluble material (chiefly quartz) in the phosphate rock. Each LCC presented in Table I is computed for the 14 coarser samples exclusive of the seven concentrates since the concentrate samples appear to have anomalous reflectivities upon comparison with the coarser grades. Only the most significant LCC for each element is presented in graphical form. Discussion of Data Iron: [Fig. 1] is a graph of the relationship between iron and reflectivity (LCC = - 0.98). A good correlation with Fe2O3, is expected due to the relationship between the tan (or brown) color and the abundance of iron oxide, the principal mode of occurrence of iron in Florida phosphates.8 Note the location of the seven triangles which repre-

Jan 1, 1972

By Joseph A. Holmes

Although Venezuelan production attained a new peak in 1938, passing the 190 million barrel mark for the first time, there was a distinct flattening of the steep upward trend that marked 1937 and preceding years. The annual total of 190,231,780 bbl. was only 31/3 million barrels above the 1937 figure, an increase of slightly less than 2 per cent, which contrasts sharply with the 20 per cent increase of 1937 over 1936. As in the previous year, the Lake Maracaibo fields supplied approximately 73 per cent of the oil produced, Lagunillas remaining the largest single contributor in spite of a 17 million barrel decrease in its annual output. Tia Juana increased its percentage of the Venezuelan total from 14.1 per cent in 1937 to 23.4 per cent in 1938; La Rosa showed little change with 13.7 per cent; Quiriquire in eastern Venezuela was also little changed with 13.2 per cent; Mene Grande, the only other field of real importance, declined from 7.7 per cent of the total in 1937 to 6.6 per cent for 1938. Two new fields, Temblador and Bachaquero, began actively to ship oil during the year, and by November were averaging 7600 and 10,000 bbl. per day, respectively. The former is in eastern Venezuela, and the latter is the most southern of the proven Lake Maracaibo fields. (A map of Venezuela was published in Volume 127 of the Transactions.) Table 1 gives a complete résumé of Venezuelan production by fields for 1937 and 1938, and shows that 1,685,575,663 bbl. had been produced to Dec. 31, 1938. The percentage contributed by each of the principal fields to this total is shown in Table 3, as well as their trends over the past several years. From these data it is apparent that the Maracaibo Basin is the principal source of Venezuelan production, and will probably continue to hold this position for some years. At the year's end 2657 oil wells were producing, of which 2425 were in western and 232 in eastern Venezuela; 36 per cent were on natural flow, 57 ppr cent were pumping, and 7 per cent were on air or gas lift. Out of 523 wells drilled, 507 producers were completed in 1938, five less than in the previous year and nearly 100 less than in 1929. These

Jan 1, 1939

By Joseph A. Holmes

Although Venezuelan production attained a new peak in 1938, passing the 190 million barrel mark for the first time, there was a distinct flattening of the steep upward trend that marked 1937 and preceding years. The annual total of 190,231,780 bbl. was only 31/3 million barrels above the 1937 figure, an increase of slightly less than 2 per cent, which contrasts sharply with the 20 per cent increase of 1937 over 1936. As in the previous year, the Lake Maracaibo fields supplied approximately 73 per cent of the oil produced, Lagunillas remaining the largest single contributor in spite of a 17 million barrel decrease in its annual output. Tia Juana increased its percentage of the Venezuelan total from 14.1 per cent in 1937 to 23.4 per cent in 1938; La Rosa showed little change with 13.7 per cent; Quiriquire in eastern Venezuela was also little changed with 13.2 per cent; Mene Grande, the only other field of real importance, declined from 7.7 per cent of the total in 1937 to 6.6 per cent for 1938. Two new fields, Temblador and Bachaquero, began actively to ship oil during the year, and by November were averaging 7600 and 10,000 bbl. per day, respectively. The former is in eastern Venezuela, and the latter is the most southern of the proven Lake Maracaibo fields. (A map of Venezuela was published in Volume 127 of the Transactions.) Table 1 gives a complete résumé of Venezuelan production by fields for 1937 and 1938, and shows that 1,685,575,663 bbl. had been produced to Dec. 31, 1938. The percentage contributed by each of the principal fields to this total is shown in Table 3, as well as their trends over the past several years. From these data it is apparent that the Maracaibo Basin is the principal source of Venezuelan production, and will probably continue to hold this position for some years. At the year's end 2657 oil wells were producing, of which 2425 were in western and 232 in eastern Venezuela; 36 per cent were on natural flow, 57 ppr cent were pumping, and 7 per cent were on air or gas lift. Out of 523 wells drilled, 507 producers were completed in 1938, five less than in the previous year and nearly 100 less than in 1929. These

Jan 1, 1939

NAME AND OBJECT. SEC. 1. This Institute is incorporated under the Membership Corporation Law of the State of New York ; its corporate name is AMERICAN INSTITUTE OF MINING ENGINEERS; and its objects are such as are stated in its Certificate of Incorpora¬tion. ARTICLE II. MEMBERS. SEC. 1. The membership of the Institute shall comprise four classes, namely (1) Members ; (2) Honorary Members , (3) Associates , and (4) Honorary Associates Only Members and Associates residing within the United States of America, Republic of Mexico and Dominion of Canada shall be entitled to vote at the meetings of the Institute. SEC. 2 All Members, Honorary Members, Associates and Honorary Asso¬ciates of the American Institute of Mining Engineers as the same existed on the day of the incorporation of this Institute, are Members, Honorary Members, As¬sociates and Honorary Associates, respectively, of this Corporation SEC. 3. The following classes of persons shall be eligible for membership in the Institute, namely, as Members and Honorary Members, all professional min¬ing engineers, geologists, metallurgists or chemists, and all persons practically engaged in mining, metallurgy or metallurgical engineering ; as Associates and Honorary Associates, all persons desirous of being connected with the Institute who, in the opinion of the Council, are suitable. SEC 4. Every candidate for election as a Member or Associate of the Institute must be proposed for election by at least three Members or Associates; must be approved by the Committee on Membership, as prescribed in the By-Laws ; and .must be elected by the Council. Not less than three-fourths of the votes cast shall be necessary to an election Every person so elected shall become a Mem¬ber or Associate, as the case may be, upon payment of his first dues as herein¬after prescribed Each candidate for Honorary Member or Honorary Associate, must be recommended by at least ten Members or Associates ; must be approved by the Council ; and must be elected by ballot at a meeting of the Board of Direc¬tors by the unanimous vote of all the Directors present ; provided, however, that the number of Honorary Members and Honorary Associates shall not at any time exceed twenty SEC. 5. If any person elected a Member or Associate does not, within sixty days after notice of his election, accept the same and pay his initiation fee and dues for the current year, his election may be cancelled at the discretion of the Council.

Jan 1, 1910

T.P. 1958 D. H. DAVIS.*-Mr. Carris has ably pre¬sented the problems of coal preparation, particularly those brought about as the result of increased mechanical loading. Many mines are now crushing the run-of¬-mine raw coal through 12 or 15 in. immediately after it is dumped from the mine car and before it is handled by conveyors. At certain mines the removal of large slate mechanically has been solved by the installation of scalping screens consisting of bars or rails set at spacing of 12 to 15 in. on the top deck of the main raw-coal sizing screen. At the plants where these are in use, the plus 12 or I5-in. raw material contains 60 per cent or more free rock or slate, so that it is easier to pick coal than to pick rock. After the screening at 12 or 15 in. is accomplished, the oversize material is diverted to one side of the shaker, where a picker allows the refuse to pass off the shaker into a chute and guides the coal back onto the shaker. After the large rock has been removed, it is then advisable to reduce the size of rock by crushing before putting it onto a conveyor. A great saving in picking labor has been made by the use of such scalping screens, which in addition has maintained the plant capacity when handling a dirtier feed. The great increase in percentage of coal under 1/4 or 3/8 in., coupled with a greatly increased percentage of free impurities in this size, is the most serious problem that has been brought about by mechaniced loading. Many plants that formerly prepared good quality 1/4-in. to o or 3/8-in. to 0 slack by air¬cleaning are faced with installing facilities for wet-cleaning mechanical and heat-drying and water clarification. The change to wet prepa¬ration of fines usually affects the marketing problems for many coal companies. There will also be problems involving wastage of fine solids and stream pollution. Much work will be necessary for improvements in present practice. Pneumatic and electrostatic methods for cleaning fine coal should receive consider¬able attention in an attempt to avoid wet¬cleaning of fines. The preparation supervisor and the plant personnel should not be satisfied merely to run the cleaning-plant machinery and assume that the job will be done for them. Coal is a heterogeneous substance and in many instances is constantly changing. This is more true when full-seam methods are in use. Only persons trained to observe closely and make the necessary changes in plant operation will be able to solve the many problems that will be imposed on the preparation plants. The plants will require skillful and observant operating men. With full-seam mining methods, seams of roof coal will often be mined. Under the former mining systems these strata were not mined and frequently they contain a high per¬centage of bony and banded partings. The mining of this coal will greatly alter the washability and specific gravity characteristics of the feed to the plant. Often the percentage of 1.40 to 1.60 sp. gr. increased from 3.5 to 7.5 per cent, or nearly a 1.0 per cent increase in the ash content of the 1.60 sp. gr. float coal. Thus the cleaning problem is much more difficult, and it is unlikely the same ash content of cleaned coal can be produced as before without a decrease in recovery or the produc¬tion of a "middlings" product. Mr. Carris had this in mind when he said "The quality of the

Jan 1, 1946

By J. P. G. Farr, R. Brownsword

THE role of solute segregation in the formation of cellular solidification substructures in tin and its dilute alloys is well-established, see, e.g., Ref. 1. Segregation has been shown to persist during cooling, enabling solidification structures to be studied from sections taken at some distance behind the interface. In the present work, a single crystal of commercial nickel, 99.965 pct, was examined in this way. The crystal was cut from the center of a rod given a single pass in an electron beam floating zone melter. Polished sections of a nickel specimen taken normal to the growth direction showed a very fine precipitate phase, the distribution of which varied over the section. The identification of the phase proved difficult because of the small amount present and the small particle size, about 1 p: but it was shown by probe microanalysis to contain only nickel and oxygen in detectable concentrations and was probably nickel oxide, NiO. Bulk analysis of the material before melting showed there to be only 3 to 4 ppm of oxygen present, thus demonstrating a very considerable segregation concentration effect. In some areas of the section the precipitate formed a discontinuous hexagonal network suggesting decoration of the cellular boundaries known to be present in the sample2 whereas in a restricted region the precipitate formed small clusters. Occasionally it could be seen that the clusters were at the intersections of an hexagonal network of cellular dimension. It was suggested3 that this was the result of enhanced segregation to the cell boundary intersections whereas general cell boundary segregation was insufficient to give a precipitate. Enhanced nodal segregation has since been demonstrated in a number of systems.1, 4-8 The development of a suitable electrolytic etching technique (perchloric acid 20 pct v/v; ethyl alcohol 70 pct; glycerol 10 pct; current below electropolishing plateau; 1 to 2 sec etching) suggested the association of the phase with regions of solute segregation (where ko < 1); in these regions anodic attack produced grooves or depressions. In a study of the variation of solidification substructures with degree of constitutional supercooling, Biloni et a1.&apos; appear to have used standard growth conditions and varied the solute concentration. They were able to produce in a series of individual tin crystals examples of substructure ranging from planar interface through various cellular structures to den- Fig. 1—Electroetched section taken normal to the rod axis; the center of the rod lies to the left and the periphery to the right of the micrograph. The variation of structure across the section is evident. Magnification 60 times. drites. It was possible in the present nickel crystal to observe a continuous range of substructures varying with degree of supercooling across a single section as shown in Fig. 1. Growth rate, 13 mm per min, and temperature gradient were essentially constant; the variation in structure is thought to be due to a radial gradient in solute concentration ahead of the solid interface. The liquid at the interface is likely to have been richer in solute toward the periphery of the zone, the result of curvature of this interface. The type of substructure was seen to vary with increasing constitutional supercooling as follows: a) region free of precipitate. top left, Fig. 1: 6) region of nodal precipitates which became arranged in hexagons on passing from the center of the rod: c) irregular hexagonal cells with incomplete boundary precipitation; d) regular hexagonal cells of decreasing size with complete boundary precipitation. Fig. 2 shows the transition from stage 6 and Fig. 3 shows the structure in stage d. Within stage 0, the range of conditions over which irregularly positioned nodes occur appears to be small and the nodes are soon recognizable as taking up positions at the intersections of an hexagonal network as the supercooling increases.

Jan 1, 1970

By W. A. White

UNDERCLAY squeeze is the plastic flowing of underclay below coal pillars into mined-out entries and rooms. Squeezes may be caused either by wet mine conditions where the moisture is taken up by the clay—making it more plastic—or by the presence of certain clay minerals, such as mont-morillonite, which are plastic when there is enough natural moisture. Under either condition, sufficient stress will cause the underclay to flow. Squeezes may fill an entry or room within several hours, or it may be several months before movement stops. Squeeze areas commonly cover hundreds or thousands of square yards. The Coal Div. of the Illinois State Geological Survey has collected samples of underclays from various mines and from cores drilled by coal companies in the state. From these samples natural moisture content, particle size and particle size distribution, and clay mineralogy are determined. Data from samples collected from the underclay below Herrin (No. 6) coal in the Lumaghi Coal Co. mine near Collinsville, Ill., are used in this report to clarify points in the discussion. Data from samples taken from other mines lead to the same conclusions. A generalized geological section for the area is given in Table I. The underclay below coal No. 6 ranges from a few inches to 3 or 4 ft thick. The upper 6 to 18 in. are noncalcareous; the lower part becomes more calcareous with depth. Limestone nodules become larger with depth, almost grading into the limestone below. In areas where the clay is nearly absent the limestone may thicken to take its place; thus they may complement each other in thickness. There are two types of squeeze areas in a mine. In one type up to 3 or 4 ft of underclay lie in what appears to be a depression in the limestone underneath. This is suggested by a rim surrounding the squeeze area where the underclay is thin and the limestone lies within a few inches of the coal. In the second type the underclay of the squeeze area is surrounded by underclay of similar thicknesses which does not squeeze. Test Methods: Natural moisture content, particle size and particle size distribution, and clay mineralogy were determined by the following methods: Natural moisture is the moisture content a clay contains in its natural environment, expressed in percentage of the weight of ovendried clay (110°C or 230°F). To obtain the natural moisture content, given in Table 11, the clay samples were sealed in containers as soon as the samples were taken in the mines. Particle size and particle size distribution were determined by the pipette method,&apos; and the data were plotted as cumulative curves, Fig. 1, on semi-logarithmic paper. Particle size was plotted on the logarithmic scale and percentage on the arithmetic scale. The quartiles (diameters that correspond to frequencies of 25 and 75 pct) and medians (diameters that correspond to the frequency of 50 pct) of the samples were determined from these curves. The clay minerals were identified from the data obtained by differential thermal&apos; and X-ray powder" techniques. The differential thermal analyses were made on the whole samples, whereas the X-ray analyses were made on fractions of less than 2p. Data and Discussion Moisture Content: After the sealed jars had stood for 24 hr, those that contained squeeze samples had perspired, so that droplets of water had accumulated on the insides of the jars. Table II shows the moisture in the clay after it had perspired for 24 hr. (This perspiring was not noted in samples from nonsqueeze areas.) After perspiration one of the squeeze samples still had a higher moisture content than the samples that did not squeeze. Clay Mineralogy: The thermal analysis, Figs. 2 and 3, indicates that the clay minerals are chiefly micaceous in type; the low-temperature endothermal

Jan 1, 1957

By R. S. Rickard, M. C. Fuerstenau

Anodic polarization curves for iron dissolution and cathodic polarization curves for copper deposition and ferric and hydrogen ion reduction were studied. These results were used to predict the relative rates of the reactions: The rates of the first two reactions were found to be first order with respect to the reacting ion, and the rale-controlling step was diffusion of the ions to the callzode surface. The rate of hydrogen ion reduction in an oxygen-free solution is dependent on the reciprocal of the square root of the hydrogen ion activity. In solutions containing oxygen, the rate of hydrogen reduction becomes dependent on the square root of the partial pressure of oxygen. At equal concentrations copper precipitation occurs about twice as fast as ferric ion reduction. In an air-saturated solution containing 0.01 M cupric ion at pH 2, the rate of hydrogen ion reduction zs about 10 times slower than that of copper precipitation. At pH values below 3, the rate of hydrogen reduction in oxygen-free solutions is very slozu. COPPER cementation has been utilized industrially for many years as a means of recovering copper from aqueous solutions. There are many different types of cementation plants, but all simply provide a means of contacting iron with relatively dilute copper solutions. In the past little or no attention has been paid to rates or mechanisms of the reactions involved. As a result, this and other studies&apos;-3 have been undertaken recently to establish the important parameters in this system. The reactions involved in copper cementation by iron are: Since transfer of charge is involved in every case, these reactions should be considered from an electrochemical point of view. In any electrochemical system involving electrolytic conduction, passage of electrons necessitates ion transfer to the respective electrodes according to Faraday&apos;s law. The current in the system will be proportional to the rate of ion transfer, and, therefore, when the current in the galvanic cell is known, the rates of the reactions involved can be determined. Galvanostatic electrode measurements5" are applicable for these electrochemical studies, in that with this technique polarization curves (current density vs electrode potential) are established by impressing a constant current through an electrode and measuring the electrode potential. Once the current density, electrode potential, and reacting area are known for each reaction in this cementation system, the rates of the iron-consuming reactions can be determined. EXPERIMENTAL MATERIALS Several metal electrodes were used in this investigation; they are shown in Table I. Solutions were made with reagent-grade salts and conductivity water. Air, nitrogen, and oxygen were employed. All of these gases were saturated with water and degreased prior to use. EXPERIMENTAL PROCEDURE The experimental work was divided into two general areas. The first area involved galvanostatic measurements, which were used to determine the rates of reactions as a function of various parameters. The second area comprised actual cementation experiments to check the rates predicted from the electrode measurements. Galvanostatic Electrode Experiments. Polarization curves were obtained using a standard galvanostatic technique5&apos;= with the apparatus shown in Fig. 1. The various electrode polarization experiments were run the same way except for changes in solution composition, polarity, and type of measured electrode. The general procedure involved the following steps: 1) a solution was made 0.5 M in sulfate ion and to the desired cation concentrations; this solution was placed in a constant-temperature bath and saturated with the desired gas; 2) the electrodes were cleaned and placed in the electrode holder; 3) the previously cleaned apparatus was assembled and immersed in a constant-temperature water bath (temperature controlled to ± 0.05"C); 4) the electrode was then positioned; the solutions were introduced, and the polarization meas-

Jan 1, 1969

By G. C. Broadhead

THE lead district of Southeast Missouri covers an area of over 3000 square miles, including Maries County on the west, Jefferson on the east, Franklin on the north, and part of Madison on the south, or parts of ten counties. A general section of the rocks of the southeast part of this region would be about as follows, numbering from the top 1. Sandstone (the second of Missouri geologists), - 20 feet. 2. Cbert beds-beds of passage below, - 125 feet 3. Magnesian limestone, chert, and quartzite, - 100 to 300 feet 4. Lower magnesian limestone, - 100 to 150 feet 5. Gritstone and lingula beds, - 50 feet 6. Ozark marble beds, - 5 to 20 feet 7. Sandstone and conglomerate, - 5 to 90 feet 8. Porphyry, Archaean. 9. Granite, The thickness is approximate, for it is not possible to obtain the correct thickness of the various beds. No. 1 may be seen as de¬tached outliers or loose masses of a hard sandstone or quartzite, and is found on the hilltops in the southern part of Madison County, in like topographical position in Reynolds County and the western part of Washington County. No. 2 consists of alternations of chert, clay, and quartzite. It is the formation which contains most of the limonite deposits of Central and Southern Missouri. In Reynolds County shafts have pene¬trated it 75 feet. Outcrops there and in Madison would indicate it to be at least 125 feet thick. Fossils obtained in various places prove it clearly to be of the age of the calciferous sandrock of the New York system, and Nos. 1 and 2 may also be referred to the age of the second sandstone of Missouri. No. 3 consists chiefly of thick beds of ash, drab and flesh-colored magnesian limestone, both coarse and fine-grained. These beds, where they occur, in Washington, Jefferson, and the southern part of Madison Counties, contain a good deal of quartz in drusy cavities. In Washington County the limestones are beautifully ramified by a system of connected drusy cavities generally lined with minute quartz crystals arranged in botryoidal and mammillary forms, and called u mineral blossom " by the miners. This is the lead-bearing rock of Washington County, but in the southern part of Madison it does not appear to be galeniferous. It is also undoubtedly the equivalent of

Jan 1, 1877

By G. C. Broadhead

The lead district of Southeast Missouri covers an area of over 3000 square miles, including Maries County on the west, Jefferson on the east, Franklin on the north, and part of Madison on the south, or parts of ten counties. A general section of the rocks of the southeast part of this region would be about as follows, numbering from the top: 1. Sandstone (the second of Missouri geologists),.... 20 feet. 2. Chert beds—beds of passage below,...... 126 " 3. Magnesian limestone, chert, and quartzite,. .. 100 to 300 " 4. Lower magnesian limestone,......100 to 150 " 5. Gritstone and lingula beds,....... 50 " 6. Ozark marble beds,........5 to 20 " 7. Sandstone and conglomerate,. .. .. 5 to 90 " 8. Porphyry, Archæan 9. Granite, The thickness is approximate, for it is not possible to obtain the correct thickness of the various beds. No. 1 may be seen as detached outliers or loose masses of a hard sandstone or quartzite, and is found on the hilltops in the southern part of Madison County, in like topographical position in Reynolds County and the western part of Washington County. No. 2 consists of alternations of chert, clay, and quartzite. It is the formation which contains most of the limonite deposits of Central and Southern Missouri. In Reynolds County shafts have penetrated it 75 feet. Outcrops there and in Madison would indicate it to be at least 125 feet thick. Fossils obtained in various places prove it clearly to be of the age of the calciferous saudrock of the New York system, and Nos. 1 and 2 may also be referred to the age of the second sandstone of Missouri. No. 3 consists chiefly of thick beds of ash, drab and flesh-colored magnesian limestone, both coarse and fine-grained. These beds, where they occur, in Washington, Jefferson, and the southern part of Madison Counties, contain a good deal of quartz in drusy cavities. In Washington County the limestones are beautifully ramified by a system of connected drusy cavities generally lined with minute quartz crystals arranged in botryoidal and mammillary forms, and called " mineral blossom " by the miners. This is the lead-bearing rock of Washington County, but in the southern part of Madison it does not appear to be galeniferous. It is also undoubtedly the equivalent of

By F. E. Bash

PREVIOUS to the war, this country depended on Europe for its supply of a number of alloys of great importance in the manufacture of electrical apparatus and equipment. When this source was cut off shortly after the beginning of hostilities and the small stocks in the United States were exhausted, either inferior substitutes had to be used or the manufacture of the apparatus suspended. Since electrical equipment was of primary importance in the prosecution of the war, the substitutes had to be used until the composition and processes of manufacture of the alloys could be determined. Included among these alloys was one generally known as manganin, which is composed chiefly of copper and manganese and which, beside having a low-temperature coefficient of resistance, has a low thermal electromotive force against copper. These qualities make it valuable for the manufacture of electrical instruments and machines in which it is used in the shape of wire, rod, and strip. As a result of these circumstances, an investigation was started to deter mine how manganin could be made on a commercial basis so that a product of uniform quality and the necessary electrical characteristics could be produced. The object was to procure an alloy with temperature coefficient of resistance not greater than T 1 X 10-5 per ° C. and a thermal e.m.f. against copper no greater than that of the imported material. It is characteristic of manganin that the temperature-resistance curve is not a straight line but has a peak, which varies in position with different samples; it is most desirable, however, to have it at a temperature of 25° C. if possible. The coefficients of manganin from all records available ranged from a large negative to a large positive value. The composition as reported by different authorities is given in Table 1. Prof. Matthew A. Hunter, of Rensselaer Polytechnic Institute, made up a number of small melts of manganin in a graphite crucible and the one that he reported as having the best coefficient gave the following analysis: Copper, 83.6 per cent.; nickel 2.5 per cent.; manganese,-13.6 per cent.; iron, 0.3 per cent. An analysis of a sample of German manganin gave the following: Copper, 82.6 per cent.; nickel, 3.8 per cent.; manganese, 12.8 per cent.; iron 0.7 per cent.

Jan 9, 1919

By S. R. Elliott

The Spies mine is located in the eastern half of the northwest quarter of section 2443-35, near the village of Iron River, Mich., and is operated by The Cleveland-Cliffs Iron Co. Speaking generally, the jasper hanging walls of most of the deposits in the Iron River district dip at a steep angle and are exceedingly strong, standing without caving, even after mining has been continued for years and after large excavations have been made. The ore is fairly hard and tough and contains no slippage faces. It occurs in large masses, which are often egg shape, with the smaller end down, and can be mined in open stopes without the use of timber. The common system employed in the district is the shrinkage stope, or some modification of it. The Spies system was developed to utilize the advantages of the open-stope method and to avoid the disadvantages of the shrinkage stope. The Spies shaft was sunk to such a depth that the bottom, or third level, was in rock at a short distance below the bottom of the orebody, the shape and extent of which had been previously determined by diamond drilling. This is shown in plan and by the ore contours at the first, second, and third levels in Fig. 1, and in section in Figs. 2 to 7. In order to provide the necessary mills and raises, three parallel crosscuts were driven on 25 ft. centers on the bottom level. Drifts on the second and first levels were driven to the orebody and followed the foot wall in a southerly direction to the end of the ore. In crosscut 3, Fig. 1, raises 30, 40, 50, and 60 were carried up on the foot wall and holed into the second level, and were ultimately carried up and holed into the first level. These foot-wall raises carry the pipes and ladders, provide a means of ventilation, and furnish safe communication to all working places in the stope. From crosscuts 1, 2, and 3, raises were completed to a height of 32 ft., or the elevation of the first sublevel. They were then connected by east and west crosscuts to the main foot-wall raises 30, 40, 50, and 60, shown in Fig. 4. The crosscuts in raises 1 to 5 were then driven west and the

Jan 1, 1923

By C. Y. Garber

INTEREST in the sink-float plant operated by the Bunker Hill and Sullivan Mining and Concentrating Co. at Kellogg, Idaho, has recently been largely confined to the preparation and reconditioning of the galena medium. The ease and simplicity of these operations in a concentrating mill producing a flotation lead concentrate has occasioned enough comment to possibly justify a brief description. The subject is treated from an operator&apos;s viewpoint only; no effort is made to discuss it in a theoretical or technical manner. PLANT AT BUNKER HILL The sink-float plant was first operated in December 1941. It was built for the purpose of quickly increasing mill capacity with a minimum of equipment. It is the Huntington-Heberlein sink and float process using galena medium and is operated under license from the Sink and Float Corporation, New York city. Lead-zinc ore from the Bunker Hill mine is crushed to pass a I ¼ in. screen and is then washed and separated on vibrating screens having 4 ½ -mm. round-hole punched plates. The screen undersize, amounting to 33 per cent of the mill feed, is dewatered and sent to the ball-mill feed bins. The screen oversize goes to the sink-float plant, where 50 per cent of the oversize, or 33 per cent of the mill feed, is float, which is washed free of medium and disposed of as a tailing. The remaining 33 per cent is sink, which, after washing, is crushed to pass ½ in. and joins the undersize in the ball-mill feed bins. The normal plant capacity is 1700 tons per 24 hr. About 1.7 per cent of the total lead and 3.3 per cent of the total zinc in the feed is lost with the sink-float tailings (Table I). [ ] More complete descriptions of the H. H. process and Bunker Hill sink-float plant are given in several recent articles, listed at the end of the paper. PREPARATION OF MEDIUM AT BUNKER HILL New medium is made intermittently as needed, usually 12 hr. in each 6 days. A small portion of the current mill flotation concentrate is diverted from the lead cleaner cells to a I-in. vertical sand pump and pumped to a two-cell 36-in. Agitair flotation machine, where NaCn and ZnSO4 are added and the grade of concentrate is improved as shown in Table 2. Tailing from this operation is returned by gravity

Jan 1, 1946

By S. R. Elliott

The Spies mine is located in the eastern half of the northwest quarter of section 2443-35, near the village of Iron River, Mich., and is operated by The Cleveland-Cliffs Iron Co. Speaking generally, the jasper hanging walls of most of the deposits in the Iron River district dip at a steep angle and are exceedingly strong, standing without caving, even after mining has been continued for years and after large excavations have been made. The ore is fairly hard and tough and contains no slippage faces. It occurs in large masses, which are often egg shape, with the smaller end down, and can be mined in open stopes without the use of timber. The common system employed in the district is the shrinkage stope, or some modification of it. The Spies system was developed to utilize the advantages of the open-stope method and to avoid the disadvantages of the shrinkage stope. The Spies shaft was sunk to such a depth that the bottom, or third level, was in rock at a short distance below the bottom of the orebody, the shape and extent of which had been previously determined by diamond drilling. This is shown in plan and by the ore contours at the first, second, and third levels in Fig. 1, and in section in Figs. 2 to 7. In order to provide the necessary mills and raises, three parallel crosscuts were driven on 25 ft. centers on the bottom level. Drifts on the second and first levels were driven to the orebody and followed the foot wall in a southerly direction to the end of the ore. In crosscut 3, Fig. 1, raises 30, 40, 50, and 60 were carried up on the foot wall and holed into the second level, and were ultimately carried up and holed into the first level. These foot-wall raises carry the pipes and ladders, provide a means of ventilation, and furnish safe communication to all working places in the stope. From crosscuts 1, 2, and 3, raises were completed to a height of 32 ft., or the elevation of the first sublevel. They were then connected by east and west crosscuts to the main foot-wall raises 30, 40, 50, and 60, shown in Fig. 4. The crosscuts in raises 1 to 5 were then driven west and the

Jan 1, 1923