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By John W. Langley

In the summer of 1888 it was the fortune of the writer to present the subject of the desirability of establishing a set of samples of steel, which should be analyzed with extreme care, in order that they might become standards to which scientific and commercial analyses of iron and steel could be subsequently referred; also, that greater uniformity in the results of analyses might be brought about, since these standards would bear towards analytical methods somewhat the position which the original units of weight and length, the gramme and meter, or the pound and yard, preserved in Paris, London, and Washington, do to the mechanical arts. The plan met with hearty co-operation, with the result that com mittees were appointed in Sweden, Germany, France, England, and America, to receive the material and to see that the necessary au alyses were executed. In England, the British Association for the Advancement of Science appointed a committee, which subsequently published a plan

Jan 1, 1891

By William Mikulas

LITTLE work has been done in the field of the nickel-tin binary system. The complete diagram has been investigated on two occasions, but the results are in very poor agreement. The structure of a compound NiSn, and the solubility of tin in nickel have been determined by X-ray methods. Several investigations have been made of the liquidus curve, and the compositions of the eutectics have been determined. A study of the literature, however, shows that there is no satisfactory agreement between the data presented in the various papers. The present investigation was undertaken in an attempt to determine the equilibrium conditions, and to correlate X-ray with metallographic data. The equilibrium diagram was determined by thermal and metallo-graphic means, and the solubility of tin in nickel further investigated with X-rays. Powder diagrams were made of the intermetallic com-pounds, and three of the structures were partly determined. No attempt was made to determine the range of homogeneity of the inter-metallic compounds.

Jan 1, 1937

THE CHAIRMAN (F. K. COPELAND,* Chicago, Ill.).-At this particular time conditions existing in this, country, and elsewhere, make all questions of milling or smelting or mining, or anything else, absolutely secondary to the one question of labor. We have always devoted our attention largely to the efficiency of machinery, and to reductions in costs, etc., and have let this tremendous problem of our relation to labor more or less take its own chances. There has never been a time when those who are responsible for the operation of business of different kinds were as com-pletely at a loss as they are now, so that anything that can be brought out that relates to labor is, to my mind, of utmost importance. T. T. READ, Washington, D. C.-This formulation of a method of curtailing forces at the Copper Queen is a notable step in advance of our treatment of personnel in the mining industry. So far as I know, it is the

Jan 12, 1919

By S. L. Hoyt

ABOUT three years ago eight standard steels were prepared for the cooperative investigation of methods for oxygen analysis, sponsored by the Iron and Steel Division of the American Institute of Mining and Metallurgical Engineers and by the National Bureau of Standards. A preliminary report of the results was made at the annual meeting of the A.I.M.E. in February, 1936. ? This report showed the reliability of vacuum-fusion methods and further brought out certain advantages of the fractional vacuum-fusion method. The results obtained by the authors with the latter method will be discussed here, with some com-ments on the procedure for those who are interested in determinations of gases in steel. Some additional comments are offered on the use of the polarizing microscope for identifying the inclusions in the steel to check and amplify the findings of the fractional vacuum-fusion analysis. For details of the fractional method, see the paper by L. Reeve1.

Jan 1, 1937

Executive Committee, Board of Directors Augustus B Kinzel, Chairman, J L Glllson, Vice-Chairman, A W Thornton, Howard C Pyle, Grover J Holt Finance Committee, Board of Directors Andrew Fletcher, Chairman, J S Vanick, Gall F Moulton Investments Gail F Moulton, '60, Chairman, Henry Krumb, '59, J Loveloy, '61, C R Dodson, ex off as Treasurer, Andrew Fletcher, ex off as Chairman, Finance Com¬mittee Endowment Andrew Fletcher, Chairman, N G Alford, H DeWitt Smith, W J Coulter, J V N Dorr, R B Gilmore, J B Haffner, O H Johnson, D H McLaughlin, J R McMillan, L F Reinartz, C E Weed, Wilfred Sykes, J R Suman Honorary Memberships H DeWitt Smith, '59, Chairman, C E Reistle, Jr, '59, Grover J Holt, '59, L F Reinartz, '59, M L Haider, '60, D H McLaughlin, '61, John M Lovejoy, '62, Augustus B Kinzel, ex off as President

Jan 1, 1958

By N. F. Schulz, H. A. Lex

Representative samples of typical manganiferous iron ores from the Cuyuna Range, Minn., were reduced to the metallic iron state at temperatures just short of fusion with an excess of coke in the manner prescribed by the R-N Direct Reduction Process. The magnetic separation characteristics of the reduced ores were determined at several grinds by means of the Davis magnetic tube concentrator. The efficiency of metallic iron concentration by magnetic separation was a direct function of the degree of metallization of the ore sample and of the degree of liberation at-tained in grinding. Some improvement of liberation characteristics was observed if a small amount of sodium chloride was present in the ore during reduction. Despite the extremely fine-grained structure of the crude ores, iron concentrates containing more than 90% Fe at iron unit recoveries of 90% or more were obtained from well-metallized samples of three of the four ores tested. The rejection of manganese to the tailings corresponding to such separations varied from 80% to 95%. The manganiferous iron ores of the Cuyuna Range in Minnesota constitute a major potential source of manganese in the United States provided that a technically and economically feasible process can be devised for its recovery. The iron and manganese of these ores occur chiefly as oxides or carbonates in the form of very small, irregular, discrete grains embedded in a matrix of quartz or other siliceous gangue. The present investigation was undertaken as a sequel to an earlier one conducted jointly by the U.S. Bureau of Mines and the R-N Corp. Those results indicated that the R-N Direct Reduction Process might be a means for recovering both a metallic iron concentrate and a marketable manganese by-product from Cuyuna manganiferous iron ores.' The R-N Process is one of many proposed schemes for the treatment of crude iron ores involving the di- rect reduction of the iron content to metallic iron followed by physical extraction of the iron. In general, it consists of the following stepsz2 1) Iron oxide in crushed natural ores or iron concentrates is about 95% reduced to metallic iron at elevated temperatures but without fusion in a rotary kiln in the presence of a solid carbonaceous fuel (usually coke), limestone, and combustible gases. 2) The kiln product, consisting of metallized ore, excess coke, lime, and coke ash is cooled. The excess coke is recovered and recycled to the kiln feed. 3) The metallized ore is ground for liberation and magnetically separated to yield a metallic iron concentrate. 4) The metallic iron concentrate is agglomerated by a briquetting process. The reduction kiln temperatures must be high enough for the desirable chemical reactions to proceed at practical rates without causing fusion of any of the ore constituents. The time of exposure of the ore to the reducing conditions must be ample for 90% to 95% metallization of the iron oxides present. If more than 95% of the iron is metallized, however, difficulties may arise in the briquetting step, presumably because of accompanying higher carbon content of the metallic iron. Although not always necessary, powdered limestone or dolomite may be added at some time during reduction to aid in eliminating sulfur and phosphorus from the final product.3,4 Other additives, notably sodium chloride, when present during reduction, result in improved liberation characteristics of the metallic iron from certain reduced ores.'v6 Under the reducing conditions normally employed, P(co + H2)= 1 atmosphere, and 1830' to 2150°F (1000° to 1170°C), the R-N Process is claimed to be adaptable to a wide variety of low, medium, and high grade iron and manganiferous iron ores. The manganese oxides and carbonates are reduced mostly to nonmagnetic MnO which is rejected to the nonmagnetic tailings. Manganese-bearing pyroxenes of the original ore, however, may be rejected poorly, if at all, apparently because these minerals occur within the iron lattice or are entrapped in the metal particles.7 The investigation was limited to studies of the Cuyuna ores listed in Table I, which were reduced to the metallic iron state under various conditions

Jan 1, 1969

By F. Weinberg

Measurements have been made of solute segregation during dendrilic growth by using radioactive solute elements and ,measuring the activity of den(12-ites cut from decanted specimens. This has been done for both lead awl tin based binary alloys contaitzing the following solute additions: Ag, T1204, was dependet on ko, the equilibrium distribution coefficient in the following way Fay k &apos;c 0.1, C/C 0.6; for k0 >0.1. 0.6 <c,/c,< I. Qualitative obse?-vations were madc of dendritic segregation, by using autoradiographic techniques, for the Sn + Ag110 and Sn + Tlo4 systems. The observation were found to he in general agreement with the measurements ofCA/Co. Autoradiographic were also obtained of scctiolccl delzr11-iie stalks. These indicated that the stalks had a substructure, dclileated by solute corzetlt?atio?zs nlolg the substructure walls. A new dendrite growth direction <JI2> is reported for tila. SOLUTE segregation in dilute binary alloys has been investigated by Pfann,&apos; Smith, Tiller, and Rut-ter,&apos; and others. They considered the case of a slowly advancing plane solid interface, and derived expressions for the distribution of solute in both solid and liquid during solidification. To determine these expressions, they assumed no diffusion in the solid and either complete mixing in the liquid:&apos; or diffusion controlled solute movements in the liquid without any convective mixing.&apos; The present investigation considers solute segregation during dendritic growth, in which case the solid-liquid interface is not plane, and the growth rates are rapid. Segregation under these growth conditions has not been treated mathematically, because of the relative complexity of the system. It has been suggested by Chalmer, on the basis of preliminary results, that an alternative to the diffusion and heat flow controlled conditions during growth is &apos;diffusionless" dendritic growth in which solid is formed with the same composition as the liquid. He suggests this type of growth may depend upon a solvent-solute relationship that permits some solid solubility without excessive increase in internal energy, as is the case for solutions of tin in lead. On the other hand, Montariol,4 and others, have shown experimentally that some segregation does occur during dendritic growth in metals using etching and radioactive tracer techniques to indicate the concentrations of the solute. The present investigation was undertaken to determine, both qualitatively and quantitatively, the extent of solute segregation associated with dendritic growth in a series of binary alloys, as a function of solute concentration. PROCEDURE The solvent materials used were Vulcan Electrolytic tin (99.997 pct purity) and Tadanac lead (99.998 pct purity). The solute materials were Zn, Sn, and Sb (better than 99.998 pct purity), Ag and Co (99.5 pct purity), and T1 (Fisher "purified" metal sticks). Activation of the solute metals was carried out in the reactor at Chalk River, Canada. Master alloys were prepared by induction heating from the radioactive solute metal and the pure solvent, under argon, in graphite crucibles. Pieces of these alloys were then added to the solvent to give the required solute concentration. Dendrites were grown in essentially the same manner as that described by Weinberg and Chalmer, , in which controlled orientation single crystals were grown dendritically in horizontal graphite boats, and the liquid decanted. The crystals were grown and decanted in an atmosphere of tank argon. Before decanting, a sample of the liquid was drawn up in a glass tube and allowed to solidify rapidly. The orientations of the single crystals were such that <loo> was parallel to the growth direction, and (100) in the horizontal plane for lead, and [1101 and (110) respectively for tin. With these orientations long dendrite stalks formed along the bottom of the boat in the dendrite direction (<100> for lead and [I101 for tin) from which secondary branches grew. Only these secondary branches, which grew freely in the liquid from the dendrite stalk to the liquid surface, were used in the measurements. Accordingly, effects due to substrates and oxides on the surface of the liquid need not be considered. In order to measure the solute concentration C, of the dendrites, individual dendrite stalks were cut from the decanted specimens, remelted, and formed

Jan 1, 1962

By W. J. Moore, E. M. Swiggard, H. Shenker

Beryllium is the most soluble of the double-acceptor impurities in germanium; the solubility is at least 1 x 10 19 atoms cm3. Photoconductive, optical, and electrical measurements were made on a set of Ge:Be samples grown without other intentionally added imp~ivities. The excited-states spectrum of beryllium in germanium was determined both in zero field and in magnetic fields up to 30 kc. It was found that the absorption 0-f lines in the vicinity of the G line increased markedly with increasing magnetic field. The ioniza-tion energy of neutral beryllium in germanium was determined to be 24.3 * 0.1 mez: using the excited-states spectrum. An infrared detector using a Ge:Be element was found to have a normalized detectivity D* (50 p, 1000 cps, 1 cps) of 9 X ldO cm-~ps"~-w-&apos;. The Ge:Be sambles exhibited low-field breakdown and inibzirity band conduction effects at low temperatures. WHILE the properties of most dopants in germanium have been thoroughly investigated, the properties of beryllium in germanium have had relatively little attention. Much of the work that has been done&apos; has been concerned with the properties of singly ionized beryllium in germanium. The purpose of the present work was to determine the photoconductive and electrical properties of beryllium-doped germanium (Ge:~e) with a small concentration of other electrically active impurities. Ge:Be is of special interest since beryllium is the most soluble of the known double-acceptor impurities in germanium. MATERIALS PREPARATION A set of &:Be crystals with beryllium concentrations between 5 x 1013 and 1x 10&apos;&apos; cmm3 and without other intentionally added impurities was grown in a hydrogen atmosphere by the horizontal zone-refining techniques described by Swiggard and Shenker.2 The segregation coefficient of beryllium in germanium was found to be about 0.07 and its maximum solubility was found to be greater than 1 x 10&apos;&apos; atoms cm-3 which is in agreement with previous results.&apos; Most of the crystals were found to have a small net concentration of shallow acceptors; for example, a crystal having a beryllium concentration of 1.1 X 1016 cm-3 was found to have a net concentration of shallow acceptors of less than 1.5 X 1013 cm-3. Ingots designed to have a beryllium concentration of 1 x 1017 cm-3 or less exhibited a loss of electrically active beryllium. That is, the beryllium concentration was lower than expected and the decrease of the beryllium concentration along the length of the ingot was much larger than expected. It is hypothesized that this effect is due to the oxidation of the beryllium by the residual oxygen in the system. This effect is similar to but not as severe as the effect observed with boron in germani~m.3, 4 OPTICAL ABSORPTION SPECTRUM The excited-states spectrum of neutral beryllium atoms in germanium was studied by measuring the infrared optical absorption spectrum. A typical spectrum is shown in Fig. 1; the labeling of the absorption lines follows that of Fisher and Fan.* The spacings between the observed lines and the D line are nearly equal to the corresponding spacings for the other ac -ceptors in germanium.5-7 By the use of the theoretical result67&apos; that the neutral impurity ionization energy is 2.53 mev larger than the energy of the D line, the ionization energy of neutral beryllium in germanium was determined to be 24.3 * 0.1 mev at 4.2"K. This method yields a more precise value of the impurity ionization energy than the usual Hall effect method.&apos; The absorption spectrum of Ge:Be was also measured as a function of magnetic field using a magnetic field parallel to the incident radiation and using unpolarized radiation. A typical spectrum taken at 30 kG is shown in Fig. 2. An unexpected observation is that the absorption of the lines in the vicinity of the G line (there is a strong possibility that some of these lines may be associated with lines other than the G line) increases with magnetic field. RESISTIVITY AND HALL DATA Measurements of Hall voltage vs temperature were made on several of the samples. The thermal activa-

Jan 1, 1968

By Margaret V. Doyle, R. W. Powers

INTERNAL friction measurements, carried out as functions of temperature, have been used extensively to obtain data on the mobility of interstitial impurities in the Group V metals, vanadium, colum-bium, and tantalum. For a given frequency of vibration, the internal friction peaks at a temperature which depends principally on the particular metal and interstitial impurity. Relaxation times and corresponding activation energies are determined from a knowledge of such peak temperatures for various vibration frequencies. These experimentally determined relaxation times are related to the average jump frequencies of the interstitial impurity atoms using the model of Snoek1 and can be related to macroscopic diffusion coefficients as shown by Polder.2 In these Group V elements, the impurity whose diffusion rate has been the hardest to pin down by the internal friction technique has been carbon. The experimental difficulties associated with carbon in these metals were not evident in the earliest investigation carried out by Ke on tantalum.3 The carbon peak was thought to occur near 140°C at 1 cps on the basis of the enhancement of the height of this peak measured on specimens which had been coated with colloidal carbon and heated in vacuo at 1200°C. Presumably on the basis of similar evidence, Wert identified a peak also near 140°C at 1 cps in columbium with the diffusion of carbon in that element." Later, the difficulties of admitting carbon into these metals without simultaneously introducing oxygen were pointed out by Ang and Wert- nd by Marx, Baker, and Sivertsen.6 The latter suggested that the peaks attributed to carbon in tantalum and columbium might arise from the presence of traces of oxygen, adventitiously absorbed during the carburization. Such suspicion was confirmed, at least in tantalum, when it was found possible to prepare C-Ta specimens without contamination by oxygen. Specimens sci prepared, aitnough high in carbon content, gave no evidence of a damping peak near 140°C.7 Recently, the authors were able to Show that carbon diffuses in tantalum at a rate only slightly slower than that for nitrogen.8 At 1 cps, the carbon peak lies at 34g °C, only a few degrees above the nitrogen peak at 341 °C. However, the two could be distinguished by a different stability with respect to aging at 400 °C and by a different dependence of peak height on solute concentration. On the basis of this experience with tantalum, it appeared worthwhile to search also for a carbon peak in columbium in the vicinity of the nitrogen peak." In this report, the location of the carbon peak in columbium is made known and its position relative to the nitrogen peak is compared with the authors&apos; previous findings in tantalum. In addition, a second source of internal friction seen only in specimens of very high purity is discussed. Columbium was obtained from the Fansteel Metallurgical Corp. as either 30 or 40 mil diam stock. The manufacturer gives the following analysis as typical of this material: 99.4 pct minimum Cb, 0.10 pct maximum C, 0.5 pct Ta, 0.04 pct Ti, 0.02 pct maximum Si, and 0.01 pct maximum Fe. Wires 13 in. long were degassed near 2200°C for 4 to 16 hr in an ultimate vacuum better than 2.10" mm Hg in an apparatus described previously.8 This treatment reduced the oxygen and nitrogen damping peaks observed in the as-received material to less than 0.0001 in Q-1 above background. The latter value varied somewhat from specimen to specimen in the range 0.0004 to 0.0008, depending chiefly on the wire diameter and the frequency of vibration. The high temperature evacuation left the specimen in a rather soft condition, the Vhn being reduced to 40 from a value near 121 in the as-received conGi~iur~. The gram size was about the diameter of the specimen. After outgassing, specimens were loaded with carbon by absorption of such hydracarbons as methane or ethylene. Carbon was also added to a few speclrnens by heating them at

Jan 1, 1958

By R. C. Ferguson, Harlowe Hardinge

Oscar Johnson—In my opinion, the effect of mill speeds on grinding costs must be studied along with capital investment and dollars gathered together as profits. Comparing the entire groups of operators with those who have had the opportunity to make slow-speed mill studies, I think you will find the latter small in numbers. Most managers want the equipment worked to its maximum output. There are, however, some installations where plant and mill sizes are such that they can do the job with reduction of mill barrel speeds. The past and the present installations of the industry are laid out to get the most capacity for the least capital outlay. This is the case even with the plants of Chile Exploration, International Nickel, Morocco, and Anaconda, now under construction or being changed. The industry recognizes that most all equipment it buys today is good and can be depended upon for efficient performance. Under this scheme of things, I am doubtful that slow-speed ball mill operation will be generally applicable. With reference to the U. S. Bureau of Mines laboratory tests, I think table II could have been omitted. It is inconclusive as to maximum efficiency for the low-pulp level mill on hard ore. There should be no question about this point. However, data on mill speeds can be found to substantiate various theories as well as refute them. Gow, Guggenheim, Campbell and Coghill, in their paper on Ball Milling,&apos; believe their 2 x 2 ft laboratory mill reflects results that can be expected from large mills. If so, then referring to their table 11, they state, "The conclusion to be drawn from this second series is that high speed, not exceeding 72 pct of the critical, favors capacity, as before, but that with proper conditions of operation high speeds may give as good efficiency values as low speeds. In this case the efficiency values are nearly constant. A horizontal curve would indicate that the amount of grinding was directly proportional to the power expended, and these tests suggest that such a coildition can be made to exist in commercial operations." Table II (From Paper by Gow et a1)2 Speed. Pot Critical 32 42 52 62 72 82 Capacity: Surface tons per hr (65- mesh) 266 42.1 54.4 65.9 74.3 74.1 Surface tons per hr (200- mesh) 56.1 87.4 112.7 137.1 154.2 153.0 Efficiency: Surface tons per net hp hr (65-mesh) 35.7 36.3 36.3 35.4 34.3 32.3 Surface tons per net hp hr (200-mesh) 75.3 75.3 75.1 73.7 71.0 66.0 Ore in mill, 1.b. 98 100 100 113 122 165 The field performance data, table 111, represents much effort in its collection and preparation. But, one must realize that there are many variables that effect the efficiency of grinding mill operation, and too much must not be assumed as to the effect of some specific change. Possibly with changes in mill speed, the results might be more consistent by also a change in ball rationing, type of ball, volume of ball charge,. p.ulp level and amount of pulp in the mill, pulp consisting, design of liner, circulating load, etc. Also, changes in ore character must be reckoned with when evaluating grinding performance. At present the Climax Molybdenum Corp. is running at much reduced capacity. Mr. James Duggan informs me that at mill speeds of 17 rpm, they save a $0.025 per ton on liners and $0.025 per ton in power, but, if the demand for molybdenum increased, he would go back to higher speed to obtain maximum tonnage, as the values from the increased tonnage would far more than offset the one half saving at the slower speed. The Jnspiration ran a six months&apos; test between mills running 21 rpm and 23.5 rpm. The slower mills ground 10 pct less ore with a slight saving per ton, but when the reduced plant tonnage was checked back into the actual cost figures of concentration, the high-speed mills with their greater tonnage showed considerable advantage. To be convinced of possible practical results from the predictions in the conclusions, I think we would have to rely on the analysis of expert cost accountants to furnish the necessary proof figures. Hardinge and Ferguson are to be commended for the work in preparing this paper. I am convinced that our Massco engineers should go into higher speeds with our equipment. Harlowe Hardinge (authors&apos; reply)—For one, I heartily agree with Mr. Johnson&apos;s opening statement that the effect of mill speeds on grinding costs must be studied along with capital investment and dollars gathered together as profits. It was on this basis and for this reason the paper was written. Mr. Johnson, on the other hand, takes the position that, on the whole, low speeds are not justified from the economic standpoint, basing his principal reason on the fact that lower mill speeds cut mill capacities and hence reduce the gross income from the product produced. There is no denying this point. It is almost axiomatic. It is for this very reason that the overall advantage of lower mill speeds has been discounted and even overlooked. It was for this reason mainly that the paper was written in the first place. It is one thing to plan an efficient operation at the outset, basing one&apos;s figures on the tonnage requirements at the time, and it is quite another to be confronted with the problem of increasing the output of an existing installation at a minimum of capital expenditure. Economic consideration of a new installation is greatly influenced by referring to an old one. Too often, the analyst assumes that if this practice is followed in the new installation, one would not go wrong. It is just here that he may be wrong. Past practice and low capital expenditure are all too frequently given priority over the engineer&apos;s analysis of operating costs. When we are able to start fresh, we should give proper weight to other economic factors which do not exist in an old installation. It is these economic factors that make it possible to spend at the outset just a little more money and get it back in a matter of months and effect big savings for years to come. F. C. Bond—This paper is of considerable importance in that it emphasizes a modern trend to operate ball mills at somewhat slower speeds than formerly. We have checked the data in the paper with that obtained

Jan 1, 1951

By Harlowe Hardinge, R. C. Ferguson

Oscar Johnson—In my opinion, the effect of mill speeds on grinding costs must be studied along with capital investment and dollars gathered together as profits. Comparing the entire groups of operators with those who have had the opportunity to make slow-speed mill studies, I think you will find the latter small in numbers. Most managers want the equipment worked to its maximum output. There are, however, some installations where plant and mill sizes are such that they can do the job with reduction of mill barrel speeds. The past and the present installations of the industry are laid out to get the most capacity for the least capital outlay. This is the case even with the plants of Chile Exploration, International Nickel, Morocco, and Anaconda, now under construction or being changed. The industry recognizes that most all equipment it buys today is good and can be depended upon for efficient performance. Under this scheme of things, I am doubtful that slow-speed ball mill operation will be generally applicable. With reference to the U. S. Bureau of Mines laboratory tests, I think table II could have been omitted. It is inconclusive as to maximum efficiency for the low-pulp level mill on hard ore. There should be no question about this point. However, data on mill speeds can be found to substantiate various theories as well as refute them. Gow, Guggenheim, Campbell and Coghill, in their paper on Ball Milling,&apos; believe their 2 x 2 ft laboratory mill reflects results that can be expected from large mills. If so, then referring to their table 11, they state, "The conclusion to be drawn from this second series is that high speed, not exceeding 72 pct of the critical, favors capacity, as before, but that with proper conditions of operation high speeds may give as good efficiency values as low speeds. In this case the efficiency values are nearly constant. A horizontal curve would indicate that the amount of grinding was directly proportional to the power expended, and these tests suggest that such a coildition can be made to exist in commercial operations." Table II (From Paper by Gow et a1)2 Speed. Pot Critical 32 42 52 62 72 82 Capacity: Surface tons per hr (65- mesh) 266 42.1 54.4 65.9 74.3 74.1 Surface tons per hr (200- mesh) 56.1 87.4 112.7 137.1 154.2 153.0 Efficiency: Surface tons per net hp hr (65-mesh) 35.7 36.3 36.3 35.4 34.3 32.3 Surface tons per net hp hr (200-mesh) 75.3 75.3 75.1 73.7 71.0 66.0 Ore in mill, 1.b. 98 100 100 113 122 165 The field performance data, table 111, represents much effort in its collection and preparation. But, one must realize that there are many variables that effect the efficiency of grinding mill operation, and too much must not be assumed as to the effect of some specific change. Possibly with changes in mill speed, the results might be more consistent by also a change in ball rationing, type of ball, volume of ball charge,. p.ulp level and amount of pulp in the mill, pulp consisting, design of liner, circulating load, etc. Also, changes in ore character must be reckoned with when evaluating grinding performance. At present the Climax Molybdenum Corp. is running at much reduced capacity. Mr. James Duggan informs me that at mill speeds of 17 rpm, they save a $0.025 per ton on liners and $0.025 per ton in power, but, if the demand for molybdenum increased, he would go back to higher speed to obtain maximum tonnage, as the values from the increased tonnage would far more than offset the one half saving at the slower speed. The Jnspiration ran a six months&apos; test between mills running 21 rpm and 23.5 rpm. The slower mills ground 10 pct less ore with a slight saving per ton, but when the reduced plant tonnage was checked back into the actual cost figures of concentration, the high-speed mills with their greater tonnage showed considerable advantage. To be convinced of possible practical results from the predictions in the conclusions, I think we would have to rely on the analysis of expert cost accountants to furnish the necessary proof figures. Hardinge and Ferguson are to be commended for the work in preparing this paper. I am convinced that our Massco engineers should go into higher speeds with our equipment. Harlowe Hardinge (authors&apos; reply)—For one, I heartily agree with Mr. Johnson&apos;s opening statement that the effect of mill speeds on grinding costs must be studied along with capital investment and dollars gathered together as profits. It was on this basis and for this reason the paper was written. Mr. Johnson, on the other hand, takes the position that, on the whole, low speeds are not justified from the economic standpoint, basing his principal reason on the fact that lower mill speeds cut mill capacities and hence reduce the gross income from the product produced. There is no denying this point. It is almost axiomatic. It is for this very reason that the overall advantage of lower mill speeds has been discounted and even overlooked. It was for this reason mainly that the paper was written in the first place. It is one thing to plan an efficient operation at the outset, basing one&apos;s figures on the tonnage requirements at the time, and it is quite another to be confronted with the problem of increasing the output of an existing installation at a minimum of capital expenditure. Economic consideration of a new installation is greatly influenced by referring to an old one. Too often, the analyst assumes that if this practice is followed in the new installation, one would not go wrong. It is just here that he may be wrong. Past practice and low capital expenditure are all too frequently given priority over the engineer&apos;s analysis of operating costs. When we are able to start fresh, we should give proper weight to other economic factors which do not exist in an old installation. It is these economic factors that make it possible to spend at the outset just a little more money and get it back in a matter of months and effect big savings for years to come. F. C. Bond—This paper is of considerable importance in that it emphasizes a modern trend to operate ball mills at somewhat slower speeds than formerly. We have checked the data in the paper with that obtained

Jan 1, 1951

University of Alabama University, Alabama Mining and Metallurgical Society WILLIAM R. HIGGS, President ROBERT E. MEAD, Secretary J. R. CUDWORTH, Faculty Sponsor MILTON H. FIBS, Counselor University of Arizona Tucson, Arizona Miners&apos; Society LEE BLESSING, President R. W. CORY, Secretary E. P. MATHEWSON, Faculty Sponsor B. R. HATCHER, Counselor University of California at Los Angeles Los Angeles, California Student Chapter, A.I.M.E. ARCHER WARNE, President ROBERT JOHNSTON, Secretary E. K. SOPER, Faculty Sponsor EMILE HUGUENIN, Counselor Colorado School of Mines Golden, Colorado Student Chapter, A.I.M.E. J. Ross REED, President ANDREW PERRY, JR., Secretary J. BURNS READ, Faculty Sponsor A. W. NEWBERRY, Counselor

Jan 1, 1936

By R. W. Baldwin

On page 309, column 1, the second equation should read: Ma-M1 = dlog_Pa M2-M1 d log P2

Jan 1, 1961

By L. D. Jaffe, R. K. Pitler

IT would clearly be advantageous to produce molten titanium, suitable for alloying and casting, directly from the relatively inexpensive tetra-chloride, without using a metallic reducing agent. Accordingly, a preliminary investigation has been made of the production of titanium by hydrogen reduction of the tetrachloride in an electric arc furnace. For the reaction: TiCl4(g) + 2H2(g) ? Ti(s) + 4HCl(g), Lockhart and his colleagues&apos; have calculated equilibrium constants at 800" to 1500°K, based on tables of Brewer.&apos; Extrapolating these data on the assumption that the heat of reaction varies linearly with temperature, and using Brewer&apos;s value for the heat of fusion, there is obtained for the reaction: TiCl4(g) + 2H2(g) ? Ti(l) + 4HCl(g) an equilibrium constant at 2100°K (100" above the melting point) Kp = (PHCl)4/pTlcl4 (Ph2)2 = 0.167 atm. If this is correct, starting with hydrogen saturated with TiC14 at 25°C, where the vapor pressure of the latter3 is 12.6 mm, and maintaining the overall pressure at 1 atm, 99 1/4 pct of the TiC14 would be reduced to Ti at equilibrium. An arc furnace designed for the melting of titanium and lined with water-cooled copper was used for the preliminary experimental check. Its inside diameter was 2 7/16 in. and height 6 in. The water-cooled electrode was tipped with 3/4 in. diam tung-sten. In the one run carried out, the furnace was charged with a starting batch of 293.35 g of scrap titanium,&apos; analyzing 99.24 pct Ti. After the system was twice pumped out and flushed with argon to remove air, the arc was struck in argon and kept at 400 amp dc, electrode negative, for 1 min to melt the starting batch. Commercial tank hydrogen, dried by passing over silica gel and bubbled through technical grade TiC14 at room temperature, was then admitted to the furnace. The inlet tube directed this gas downward toward the arc and melt; the gas outlet was at the top of the furnace. The quantity of gas passed through was not measured accurately but is estimated to be about 50 liters per min at a few mm of mercury above atmospheric pressure. The arc was held in the H2-TiC14 mixture at 400 amp with little difficulty. After 10 min the arc burned through the copper lining above the melt, admitting water and ending the run. (This had happened frequently in straight melting runs under argon, and is not thought due to the atmosphere used.) In the furnace were found an ingot, several small pieces, and a little metallic powder, evidently formed when water entered the hot furnace. Some titanium also clung to the electrode. The portions were weighed and separately analyzed for titanium. Their total weight was 321.76 g of 94.82 pct overall purity. Much of the impurity consisted of tungsten broken off when the titanium was removed from the electrode. No detailed impurity analysis was made because the starting materials were impure and flooding the furnace introduced further contamination. Thus, the metal recovered contained 305.08 g Ti, as compared to 291.12 g in the starting batch. Titanium could not have been carried over from previous melting runs in the furnace, as the interior was sandblasted and the electrode ground clean before the run. Evidently at least 13.96 g of Ti were produced from TiCl4. Since this would require complete reduction of 430 liters of TiCl, gas at 12.6 mm of Hg, the efficiency of the process must have been rather high. Experimental work is continuing. No reason is seen why the process could not be scaled up to the size of a 30-ton steel-melting arc furnace. In a large unit there would be a large molten pool from which liquid metal could be withdrawn for alloying and casting. The problems of electrodes and power supply are similar to those arising in arc furnaces for melting titanium. Unreacted TiC14 and the HC1 in the exhaust gases could be recovered; unreacted H2 could be dried and re-used. The melt would be saturated with hydrogen, whose solubility in liquid titanium is unknown. Small amounts of hydrogen seem to have little effect on the properties of titanium.5 If the amount introduced was so large as to impair properties or cause casting difficulties, it could be reduced by holding the melt under an inert gas or by pumping on it, prior to casting. Acknowledgment The authors would like to thank I. Preble and M. Goldman for their valuable aid in the experimental work and the thermodynamic calculations, respectively. References 1R. J. Lockhart, J. J. Ward, M. J. Hussey, and J. W. Clegg: In unpublished report, "U. S. Air Force Project Rand. Titanium and Titanium Base Alloys." Battelle Memorial Institute (1949) 37-44. 2 L. Brewer et al: Chemistry and Metallurgy of Miscellaneous Materials—Thermodynamics. Ed. by L. L. Quill. pp 13-39, 60-192. (1950). McGraw-Hill Book Co. 3 K. Arii: Scientific Reports. Tohoku Imp. Univ. (1933) 22, 182. 4 R. S. Dean, J. R. Long, F. S. Wartman, and E. L. Anderson: Transactions AIME (1946) 166, 369-381; Metals Technology (Feb. 1946) TP 1961E. * R. I. Jaffee and I. E. Campbell: Transactions AIME (1949) 185, 646-654; Journal of Metals (Sept. 1949) TP 26813.

Jan 1, 1951

By A. U. Seybolt, V. A. Phillips

Binary iron alloys containing 1 pct of Al, Cr, Mn, Mo, Si, Ti, or V, and 0.4 pct C, 1 pct Cr steels with and without 1.2 pct A1 or 2.0 pct Ti additions, were ion-nilrided at 550° to 600° in N-H mixtures. Nitriding increased the inicrohardne ss of all the binary alloys except those containing manganese or molybdenutn, and also hardened the heat-treated steels if aluminum or titanium urns present. Transmission electron microscopy revealed particle formation in all casts where hardening occurred. Electron diffraction gare positive identifications for ALN, CrN, and a, Si3N4 in the binary alloys, and AlN and CrN in the aluminum- cold chromium-bearing steels, respectil&apos;uly. Cubic VN with a, = 4.13A was tentatively identified. Particles, apparently of CrN, also formed in the base steel but did not increase the hardness very much. Chromium and vanadium formed nitride platelets on {001}° matrix planes, while titanium gave clusters <15A diam. Aluminum nitride precipitated at grain and subgrain boundaries, and within the grains. Silicon gave profuse precipitates of several Morphologies at grain boundaries and cubical particles within the grains. No effect of the alloy carbides on nitride precipitation was observed in the heat-treated steels. THE nitriding of steel has been a well-established commercial process for about 40 years, but in spite of this comparatively long period of use there have been few studies aimed at understanding the process. Most studies, like the early but very competent work of Jones and organ&apos; and nones.&apos; were concerned with establishing the pertinent engineering variables of steel composition, gas composition, temperature, and time. As far as the present authors are aware, there have been no studies of the composition, size, shape, or distribution of the nitrides formed in the nitriding of steel. Noren and Kindbom3 did, however, examine a few nitrided steels by surface replica electron microscopy, and were able to show the presence of car-bonitrides and AlN and TiN nitrides. pitsch4,5 and Hrivnak6 examined nitrided pure iron by transmission electron microscopy. Baird7 found manganese nitrides in Fe-1.6 pct Mn when nitrided at 650°C, using the same technique. In the present work, emphasis was placed on transmission electron microscopy because of its inherently better resolution, using principally binary alloys of iron containing 1 pct of alloying element. In addition, a few simple 0.4 pct C steel compositions were examined to investigate possible carbonitride formation. It was not anticipated that all of the added elements would form nitrides under the conditions used, but it was considered desirable to obtain direct experimental evidence on this point. It would be considerably easier to ascertain the presence of alloy nitrides by examining appropriate binary alloys in preference to relatively complex steels. The work reported here could have been done using orthodox ammonia-nitriding procedures, but an operating ion-nitriding equipment was available, and was therefore used for specimen preparation. EXPERIMENTAL DETAILS 1) Materials. Binary alloys were made up from vacuum-melted electrolytic iron with 1 wt pct additions of Cr, Ti, V, Al, Mn, Mo, and Si of about 99.9 pct purity. In addition, three steels were similarly made up—a basis steel with 1 wt pct Cr and 0.4 wt pct C and two steels with further additions of 1.2 wt pct A1 or 2.0 wt pct Ti, respectively. The materials were vacuum-melted and cast as 11-lb heats into tapered square molds of about 2 by 2 in. average cross section. The castings were forged and hot-rolled to 11/4 in. rounds. Discs of 4 in. thickness by about 1 in. diam were machined from the rods. Some of these discs were hot-forged and hot-rolled to about 0.020 in. thick, sand-blasted, and then cold-rolled to about 0.003 in. thick. At this point, the surface was cleaned by light etching with HC1, then washed, dried, and vapor-degreased prior to nitriding. 2) Ion-Nitriding Procedure. The type of ion-nitriding equipment used here is similar to that described by Jones and Martin.8 Briefly, a mixture of nitrogen and hydrogen at 5 mm total pressure is placed in a vacuum chamber with a dc potential of 450 to 500 v applied between the work (cathode) and the grounded metal vacuum enclosure (anode). Nitrogen ions are accelerated to the work where a thin layer of Fe4N forms on the surface and thus sets up a nitrogen concentration gradient. This causes nitrogen atoms to diffuse into the surface layers of the alloy forming a finely divided dispersion of alloy nitrides, causing hardening of the surface. In the work to be reported here. the nitriding was carried out at 550° to 600°C to be consistent with commercial nitriding practice. The temperatures cited are those measured by a thermocouple located under a platform on which the work was sitting. Except where otherwise stated, the mixture used in nitriding the binary alloys contained -2.0 pct N, balance hydrogen. The nitrogen concentration in the nitriding gas mixture used for the binary alloys was purposely kept lower than normally used in nitriding steels. 10 to 20 pct, in order to minimize Fe4N formation. In this way only the alloy nitrides would be present as a second phase. However, in the case of steels which would contain a- carbide phase along with as

Jan 1, 1969

BECAUSE it is necessary that the powders made for casting have a magistery of salt water, I wish now to teach you to prepare the salt that must form this magistery, for without it these powders would not have the toughness to hold themselves together when they are dry. In short, you take the quantity [119v] of salt that you need to prepare and put it in a rough pot, either baked or, if it suits you better, raw but well dried. This is completely covered with a lid or is luted with well- made moulding clay. Then it is encircled with brick ends at a distance of three dita, like a drying furnace. This space is filled with good charcoal; fire is applied and it is left to stand until all the charcoal is consumed by itself* Then you take that quantity of this burned or rather melted salt which you wish to use for moistening the clay and which you think can be dissolved in the water so that it wd remain very salty. It is boiled in a pot with water and then left to stand. After it has settled, your powder is moistened with it and used for moulding. When you see by testing it that the powder stands up as you wish, it is good. If not, give it some more of this water again and continue until you see that it holds enough. For without this magistery it would return to the dryness that it had before as a powder, and you could not use it without fear that it would fall from the Games. In this way this earth, either natural or artificial, is prepared and made ready, and it is used as the need occurs.

Jan 1, 1942

By William P. Shinn

Jan 1, 1880

By Kenneth A. Gutschick, Robert S. Boynton

Lime has become a general and loosely used term to denote almost any kind of calcareous material or finely divided form of limestone or dolomite, as well as burned forms of lime. However, according to Webster, lime is only calcined limestone (known as quicklime, unslaked lime, or calcium oxide). It also embraces the secondary product of quicklime, i.e., hydrated lime or slaked lime (calcium hydroxide). There are two basic types of limestone used for lime manufacture-high calcium and high magnesium (dolomitic). The dolomitic quicklimes and hydrated limes correspond to their "high calcium" counterparts. The only difference is that the dolomitic types are a combination of the elements calcium and magnesium, in varying percents, whereas high calicum limes contain less than 5% MgO down to 1/2%. In either case a pure form of limestone of at least 97% combined carbonate content is needed to make salable lime, barring a few exceptions. The calcination of both types is diagrammed chemically as follows: [ ] In the foregoing reversible reactions the limestone is burned (calcined) in lime kilns, with the carbon dioxide content of the stone expelled as a gas. The weight loss during calcination of pure high calcium limestone is 44%; with equimolecular dolomitic limestone, the weight loss is 48%. Since lime has a strong affinity for CO_, particularly if moisture is present, it will readily revert to its original carbonate form. This occurs when quicklime "air-slakes" and adsorbs CO.. from the air. Thus, quicklime is perishable and should be stored in dry, water-tight areas. Depending upon the type of kiln used and the physical structure of the stone, the size of the quicklime may range from sandlike granules to 8 in. lumps. However, pebble sizes ranging from 1/4 in. to 2 in. are the most common. Screened quicklime fines are also com¬pressed (pelletized) into 1 in. pellets. For some purposes ground or pulverized forms of quicklime are used, ranging from No. 10 mesh to dust. Generally a pebble of quicklime is about the same size as the pebble of limestone before calcination (perhaps shrinking slightly). A more stable form of lime is hydrated lime. This is obtained by adding water to quicklime, slaking it into a dry, fine, subsieve size white powder. Because its affinity for moisture has been satisfied, it is not vulnerable to further moisture like quicklime. However, it has the same strong affinity for CO_. The following reversible chemical reactions illustrate how hydrated lime when heated (or dehydrated) can revert to the original oxide form:

Jan 1, 1975

By N. Tiner

The mechanical properties of magnesium-alloy castings are greatly improved by grain refinement, and at present considerable attention is being paid to methods of obtaining fine-grained castings. One method of achieving this end is the use of proper melting and superheating techniques. These have been employed com-rnercially to a great extent, but no comprehensive study of the subject appears to have been published at present. Numerous investigations found in the literature include some reference to superheating techniques,1"4 and Achenbach, Nippcr and Piwowarsky,% ased principally on thermal analysis, ascribe the grain-refilling action of superheating to the influence of solid foreign particles or dissolved gases present in the melt upon the course of crystallization. The primary purpose of this paper is to present the principal facts concerning the cffect of superheating on grain size of magilesium alloys. .ittempts are also made to explain the experimental results in terms of a general hypothesis. The investigations are limited chiefly to common commercial casting alloys. In order to carry on this work, it was necessary to determine the factors influencing grain size and to develop a proper technique for the preparation of samples. Thc preliminary tests made by the author indicated that the grain size of magnesium alloys resulting from the solidification of a melt is determined by alloy composition, presence of impurities, rate of cooling during solidification, thermal history of the melt and to some extent the structure of the charge used. The rate of cooling is in turn dependent upon the mass of the melt, pouring temperature, and dimensions, properties and temperature of the mold into which the melt is poured. The final grain size of the alloys is still further modified by heat-treatment subsequent to casting. It is not within the scope of the present paper to discuss all of these factors, and it would suffice to note here that when equal amounts of magnesium alloys are prepared from the same alloying materials, melted in graphite crucibles under the same thermal conditions, then cast into graphite molds at a constant temperature, the resultant solids have the same grain size. By maintaining all other factors constant, it is thus possible to vary thermal conditions of a melt and to examine the grain size of resultant castings. Preparation of Samples and Grain-size TestiNg The alloys investigated in this paper were taken from ingots made by Permanente the Or or prepared by the author with pure carbothermic magnesium and necessary alloying elements. Melting was carried out under a flux in a graphite crucible heated uniformly by an

Jan 1, 1946

By N. Tiner

The mechanical properties of magnesium-alloy castings are greatly improved by grain refinement, and at present considerable attention is being paid to methods of obtaining fine-grained castings. One method of achieving this end is the use of proper melting and superheating techniques. These have been employed com-rnercially to a great extent, but no comprehensive study of the subject appears to have been published at present. Numerous investigations found in the literature include some reference to superheating techniques,1"4 and Achenbach, Nippcr and Piwowarsky,% ased principally on thermal analysis, ascribe the grain-refilling action of superheating to the influence of solid foreign particles or dissolved gases present in the melt upon the course of crystallization. The primary purpose of this paper is to present the principal facts concerning the cffect of superheating on grain size of magilesium alloys. .ittempts are also made to explain the experimental results in terms of a general hypothesis. The investigations are limited chiefly to common commercial casting alloys. In order to carry on this work, it was necessary to determine the factors influencing grain size and to develop a proper technique for the preparation of samples. Thc preliminary tests made by the author indicated that the grain size of magnesium alloys resulting from the solidification of a melt is determined by alloy composition, presence of impurities, rate of cooling during solidification, thermal history of the melt and to some extent the structure of the charge used. The rate of cooling is in turn dependent upon the mass of the melt, pouring temperature, and dimensions, properties and temperature of the mold into which the melt is poured. The final grain size of the alloys is still further modified by heat-treatment subsequent to casting. It is not within the scope of the present paper to discuss all of these factors, and it would suffice to note here that when equal amounts of magnesium alloys are prepared from the same alloying materials, melted in graphite crucibles under the same thermal conditions, then cast into graphite molds at a constant temperature, the resultant solids have the same grain size. By maintaining all other factors constant, it is thus possible to vary thermal conditions of a melt and to examine the grain size of resultant castings. Preparation of Samples and Grain-size TestiNg The alloys investigated in this paper were taken from ingots made by Permanente the Or or prepared by the author with pure carbothermic magnesium and necessary alloying elements. Melting was carried out under a flux in a graphite crucible heated uniformly by an

Jan 1, 1946