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By T. Sterry Hunt

WET processes for the extraction of copper from its ores have of late attracted much attention, especially in Europe, where the use of oupriferous iron-pyrites as a' source of sulphur prevails. These processes present an additional interest, when, as is often the case, the copper-ore's to be treated contain one or both of the precious metals, since the complete separation of these from copper, either in the dry or the moist way, is, as is well known, one of the difficult problems of metallurgy. The principal wet processes hitherto in use for the extraction of copper from its ores, may be included under three classes : I. Those in which the copper in snlphuretted ores is rendered soluble in water by calcining them, after a preliminary roasting which removes the greater part of their sulphur, with a portion of common salt, by which the copper is converted into a chloride (Long-maid and Henderson), or with sulphate of soda, by which sulphate of copper is formed (Monnier). Allied to these is the method by which a portion of the copper is got as soluble sulphate by roasting without addition, a process which is sometimes modified and rendered more complete by re-roasting the lixiviated residues with the addition of a portion of raw sulphuretted ore (Bankart). II. Those methods in which free chlorhydric or sulphuric acid is used to dissolve the copper- from oxidized or roasted ores. These, while simple and efficient, are too costly, except in certain localities where chlorhydric acid is a waste product. Related to them is the plan which consists in exposing the oxidized and moistened ores to the slow action of sulphurous acid mixed with air, by which a soluble sulphate of copper is formed. It has been proposed to decompose the solutions of sulphate or chloride of copper by sulphuretted hydrogen, thus separating the copper as sulphide, and using the liberated acid to dissolve fresh portions of oxidized copper. It is, however, the almost universal practice to throw down the copper from its solutions, however obtained, in the metallic state by the use of iron, either scrap-iron or iron-sponge; although in some instances

Jan 1, 1882

By T. Sterry Hunt

Jan 1, 1882

By Franklin H. Sharp, Kenneth L. Clifford

During the last few years the New Lead Belt of Southeastern Missouri has become the main source of lead in the United States. It also produces significant amounts of zinc, copper and silver. The mines are located on a narrow, mineralized trend extending southward from Viburnum, MG. for about 35 miles. The ore occurs as replacement deposits in the Bonneterre lime- stone formation which is about 1000 ft below the surface. In most of the mines, enough water is produced to supply the milling requirements without any reuse. There are dry areas, however, and at least two mills must rely on water reclaimed from their tailings lake to augment the mine water. These mills have no choice but to utilize recycled mill water.

Jan 7, 1973

By William N. Poundstone

What attracts young engineering graduates into the coal industry? What do these young men expect of a career in coal mining? These questions are often asked and debated by mining men throughout the country. In order to present a comprehensive answer to them, an opinion survey was conducted at West Virginia University's School of Mines among the junior and senior classes and part of the sophomore class. The tabulation of the answers showed that the present-day mining engineering student is an older, more mature individual as compared with former years and as compared with other present-day college students. The average age of the country's record-breaking 150,000 college graduates is 24 years. Among this year's mining graduates at West Virginia University, 78% are of this age or older. Over half (54%) of those polled in the survey are married. This is com- pared to 30% as a national figure. Of those married, 38% have one child and over 6% have two children. The entire senior group covered by this survey has averaged almost three years in the armed forces. An article entitled "The Class of '49" in the June issue of Fortune magazine states that this year's class is the oldest, most mature class in history. Our survey indicates that the mining engineering students at West Virginia University are well above the average in this respect.

Jan 1, 1949

By Nelson P. Hulst

COMMITTEES. DULUTH.-Nelson P. Hulst, Chairman; J. B. Adams, W. C. Agnew, M. H. Alworth, C. W. Andrews, R. Angst, William R. Appleby, C. E. Bailey, G. G. Barnum, E. F. Bradt, Mylie Bunnell, George L. Cheesebrough, Peter Christen¬sen, F. A. Cokefair, T. F. Cole, C. A. Congdon, N. Cowling, George H. Crosby, M. D. Cullum, C. d'Autremont, Jr., H. L. Dresser, C. T. Fairbairn. Walter Fitch, F. L. Gilbert, J. T. Hale, G. G. Hartley, E. B. Hawkins, M. S. Hawkins, J. H. Hearding, Louis Hill, L. J. Hopkins, F. E. House, J. C. Hunter, 0. D. Kinney, J. W. Kreitter, E. J. Longyear, Alexander McDougal, W. A. McGonagle, A. M. Marshall, W. N. Merriam, T. D. Merrill, John Millan, P. Mitchell, Clarence Moore, Hon. Page Morris, C. H. Munger, Henry Nolte, W. J. Olcott, A. L. Ordean, Thomas Owens, F. A. Patrick, H. M. Peyton; D. M. Philbin, Capt. Charles Potter (U. S. A.), L. W. Powell, Harry Roberts, Louis Rouchleau, George A. St. Clair, J. U. Sebenius, Joseph Sellwood, Amos Shepherd, W. B. Silvey, George Spencer, George C. Stone, H. B. Sturtevant, George D. Swift, Kirby Thomas, C. D. Thompson, A. D. Thomson, G. A. Tomlinson, Charles Trezona, R. R. Trezona, Maj. J. H. Upham, Charles Van Barneveld, W. W. Walker, J. L. Washburn, A. C. Weirs, H. J. Wessinger, A. B. Wolvin, Dwight E. Woodbridge. HOUGHTON.-W. E. Parnall, Chairman; W. D. Calverley, Secretary; W. B. Anderson, L. S. Austin, Jacob Baer, William Bath, F. J. Bawden., Simon Beahan, John Been, C. H. Benedict, Walter Bloomfield, S. H. Brady, Samuel Brady, Henry Brett, A. L. Burgan, F. I. Cairns, W. H. Cake, Arthur L. Carnahan, William Carpenter, Phillip Carroll, John J. Case, T. L. Chadbourne, W. A. Childs, B. F. Chynoweth, Captain James Chynoweth, H. P. Clausen, F. G. Coggin, H. D. Conant, J. B. Cooper, J. R. Cooper, John Cuddihy, Thomas Cummings, Robert Davidson, J. B. Dee, J. R. Dee, T. S. Dee, Theodore Dengler, M. M. Dennis, Captain Thomas Dennis,. F. W. Denton, A. D. Edwards, R. M. Edwards, C. S. Fales, Daniel Fisher, Henry Fisher, James Fisher, A. L. Floeter, Frank H. Getchell, M. C. Getchell, W. M. Gibson, W. M. Gilliland, James G. Glanville, George Goodale, H. S. Goodell, A. R. Gray, Edward Grierson, Homer Guck, H. D. Haddock, Captain Josiah Hall, John L. Harris, Captain S. B. Har¬ris, Enos Harrold, F. William Hartmann, George L. Heath, C. M. Hoar, Thomas Hoatson, 0. P. Hood, Captain Thomas Hooper, Captain Joshua D. Husking, Dr. L. L. Hubbard, Arno Jaelinig, E. D. Johnson, G. A. Koenig, Edward Koepel, C. H. Krause, R. H. Leach, A. W. Leonard, James MacNaughton, Edward McCormick, Thomas McDonald, R. T. McKeever, F. W. McNair, James McRae, John Mackey, John C. Mann, Major G. A. Marr, Captain Thomas Maslin, Harry Mercer, James Merton, Michael Messner, William F. Miller, Captain J. Milligan, Dr. J. W. Moore, Charles H. Moss, H. F. Nickerson, Charles L. Noetzel, P. H. Paine, John Penrose, Captain John Pentecost, Graham Pope, R. C. Pryor, James Ramsay, J. T. Reeder, Allen F. Rees, J. H. Rice, W. G. Rice, James

Jan 1, 1905

By Kenneth R. Hancock

Iron oxides are unique in that they are the only significant colored mineral found in a natural state suitable for use as a pigment after it has been pulverized to pigmentary size. The current world production of iron oxide pig¬ments is estimated by the author to be between 450,000 and 550,000 tons based on 1969 data. The fact that highly colored natural deposits of iron ore are found throughout the world ac¬counts for its use in prehistoric man's artistic cave paintings. These early artists did not realize that they had established man's first paint test fence which now has some 20,000 years of exposure. In addition to abundance, constituting about 7 % of the earth's crust, iron oxides have the advantages of low cost, permanency, and are not toxic. Through the centuries, succeeding civilizations have utilized iron oxides as a major source for decoration and protection when coloring was desired. In the last century the chemical industry has improved on nature by developing a complete range of synthetic iron oxide pigments which surpass the pigments pro¬duced from natural iron ores in uniformity, color quality, and chemical purity. In the United States alone, the combined production of natural and synthetic iron oxides produced sales of over $28,000,000 in 1970 (Stipp, 1970). Nomenclature With the increasing importance of the syn¬thetic iron oxides it is necessary to make a distinction between the natural or mineral pig¬ments and the synthetic pigments. Natural pigments are those products which are derived from selected ores and should not be confused with iron ores mined for steel production. Iron ores that are mined for steel must be capable of being mined and reduced to iron on a com¬mercial basis. These ores are selected on the basis of iron content and processing economics. It is therefore unusual when iron ores for steel production are suitable for use as mineral pig¬ments. Natural pigment ore sources are se¬lected for their special physical-chemical prop¬erties and can command a premium price. Synthetic pigments, and in this instance iron oxides, are those pigments produced from basic chemicals. Through chemical synthesis pig¬mentary sized particles are produced as opposed to comminution, the major procedure common to all natural iron oxide pigments.

Jan 1, 1975

By L. F. Pett

ALTHOUGH Kennecott's orebody has long been outlined, it is still necessary to define further its limits. This mine, long an advocate of churn drill methods, recently supplemented its practice by using a diamond drill. So far, the diamond drill holes have been along the main canyon floor which traverses the mine area. This zone, highly fractured, is cut by numerous friable quartz veinlets encountered within the porphyry. These veinlets, formed by filling contracted porphyry fractures with hot, siliceous, mineral-bearing solutions, are often more highly mineralized than adjacent porphyry. They pulverize on contact, yielding only slight amounts of core.

Jan 7, 1951

By John G. McLain

OF all the zinc that the world consumed in 1936-'38 the United States took about 31 per cent, and almost 14 per cent of the world's zinc supply in that period was used for galvanizing purposes in the United States. Further examination of the statistics shows that about 71/2 per cent (147,500 tons in 1939) of the world zinc consumption goes into the galvanizing of sheets in the United States, which is what I am going to talk about in this paper. There is nothing especially new about galvanizing; in every year since 1921 somewhere between 41 and 49 per cent of the country's zinc consumption has been used for this purpose, and yet few people not specialists in its manufacture know much about how it is made. You take an iron or steel sheet and dip it in molten zinc and there you have a galvanized sheet-that about epitomizes popular knowledge of the subject even among engineers.

Jan 1, 1941

By W. R. Ingalls

DUPING the last two years, and especially during the last six months, a number of important articles upon the new methods for the desulphurization of galena have been published in the technical periodicals, particularly in the Engineering and Mining Journal and in Metallurgie. I proposed for these methods the type-name of "lime-roasting" of galena as a convenient metallurgical classification,' and this term has found some acceptance. The articles referred to have shown the great practical importance of these new processes, and the general recognition of their metallurgical and commercial value which has already been accorded to them. It is my present purpose to review broadly the changes developed by them in the metallurgy of lead, in which connection it is necessary to refer briefly to the previous state of the art. The elimination of the sulphur-content of galena has been always the most troublesome part of the smelting-process, being both costly in the operation and wasteful of silver and lead. Previous to the introduction of the Huntington-Heberlein process at Pertusola, Italy, it was effected by a variety of methods. In the treatment of non-argentiferous galena concentrate, the smelting was done by the roast-reduction method (roasting in reverberatory furnace and smelting in blast-furnace); the roast-reaction method, applied in reverberatory furnaces; and the roast-reaction method, applied in Scotch hearths 2 Precipitation-smelting, simple, had practically gone out of use, although its reactions enter into the modern blast-furnace practice, as do also those of the roast-reaction method.

Sep 1, 1906

By Richard W. Bayley

The Atlantic City district encompasses several districts and has been previously called by different names, e.g., Atlantic gold district, Atlantic City-South Pass mining district, and Sweetwater mining district. The district is located in a terrane of folded and faulted early Precambrian metamorphic rocks which lies near the south end of the Wind River Range in Fremont County, Wyoming, Historically it is a gold district of little production, but today is an iron district of considerable importance. Gold was discovered in placer deposits about 1842 and in quartz-arsenopyrite veins about 1867, after which there occurred a mining boom lasting a few years. Minor, intermittent gold production from placers and lodes has continued to date, but the total production has probably not exceeded a few millions of dollars. Past lode mining was generally shallow ( in the oxidized zone), the deepest about 3 60 feet. The deeper, less oxidized and sulfide ores on the same lodes have not been explored. They appear to hold the only hope for future gold mining. Sedimentary iron-formation, similar to the Lake Superior taconite, occurs in the northern part of the district. Locally, where the ironformation is thickened by folds and faults, sufficient tonnages are present to be minable, as at Iron Mountain, where the U.S. Steel Corporation produces about 1.3 million tons of iron-ore pellets annually. Exploration of the iron deposits began in 1954, and the first ironore pellets were shipped to Provo, Utah in August 1962. Indicated reserves of iron-formation (about 30 per cent Fe) are reported to be about 300 million tons.

Jan 1, 1968

By AIME AIME

EVEN the weather man joined in a friendly conspiracy to make the fall meeting of the Industrial Minerals Division at Rolla, Mo., Oct. 23-25. the splendid surges that it was. Following weeks of rain, the foliage of the Ozarks was still green, merely enlivened here and there by splashes of autumn coloring. In contrast to the tranquil beauty of the School of Mines campus under smiling Indian summer skies, the pace of the meeting was lively. Registration was larger than at any previous meeting and included an unusual number of prominent names and delegates from all over the country. From 125 to 150 were present throughout the three technical sessions, at the Thursday evening smoker, and also at the banquet on Friday; when students trooped in to the technical sessions the audience was augmented occasionally to over 200.

Jan 1, 1941

By J. Chipman, T. P. Floridis

The equilibrium of gaseous H2O-H2, mixtures with liquid iron is used to establish the activity coefficient of dissolved oxygen as log f o = — 0.20 [%O]. Discrepancies in earlier work are explained or eliminated. Additions of cobalt, molybdenum, tungsten, and platinum increase the activity coefficient of oxygen whereas copper and gold decrease it. THE importance of dissolved oxygen as a refining agent in liquid steel has led to a number of studies of its thermodynamic properties. It is the purpose of this paper to examine the effects of a number of alloying elements on the activity of oxygen in the steel bath. As a preliminary to the study of the effects of alloying elements, it seemed desirable to examine certain minor discrepancies in the published data on the properties of oxygen in simple iron-oxygen solutions. The activity and free energy of oxygen in liquid iron were studied by chipman1 in 1933 by means of the reaction h2(g)+-o = H2O (g);K; = PH2O/PH2[% O] [1] The data were in fairly good agreement with calculations from results on the similar reaction CO (g) + O- = CO2 (g); K2 =P CO2/P CO [% O] [2] which had been obtained by Vacher and Hamilton2 as an incidental part of their study of the reaction of carbon with oxygen dissolved in the melt. It was found that the equilibrium ratio k1 was not a true constant but varied with the oxygen concentration in the manner shown in Fig. 1, which is copied from the original paper. This early observation has been refuted in subsequent work but is confirmed in the present paper, and an explanation of the discrepancy can now be presented. In Fig. 1, the two points on the extreme right were disregarded in drawing the

Jan 1, 1959

By B. W. Levinger

THE system Ti-CI- has been studied by several investigators." ' Though titanium and chromium are completely miscible at high temperatures, an intermediate phase of the approximate atomic proportions TiCr, has been identified at various compositions between 60 and 68 wt pct Cr. The structure of this phase was established as the cubic C15 (MgCu2) type with 24 atoms per unit cell and a lattice parameter 6.929 kX.2 During a study of the ternary system, Ti-Mo-Cr,5 the existence of a high temperature modification of the TiCr, phase was discovered. In a series of alloys annealed at 1300°C and containing from 60 to 70 wt pct Cr and 5 pct Mo, a new phase was present which did not correspond to either ß solid solution or TiCr,. By trial, the new phase was identified to be of the hexagonal C14 (MgZn2) structure with 12 atoms per unit cell. Further work showed that the hexagonal structure was. in fact, also present in binary Ti-Cr alloys quenched from high temperatures. To make the identification more certain, the intensities of the various reflections were calculated assuming a composition TiCr2 and C14 structure. Table I lists reflection planes, interplanar distances, calculated intensities, and a comparison of these values with the lines of a binary Ti-Cr alloy (66 pct Cr) annealed for 20 min at 1385°C and water quenched. Since high angle lines were more diffuse, the correspondence between visually observed and calculated intensities was not as good at these angles. Lattice parameters were computed to be a = 4.922 kX, c = 7.945, c/a :- 1.614. The corresponding interatomic distances are: titanium to titanium distance, 3.00:, kx, chromium to chromium distance, 2.43, kX, titanium to chromium distance, 2.88,, kX. These compare to 3.00, 2.45, and 2.87 kX in the cubic phase, respectively.' The atomic positions in the C14 structure are as follows: Titanium 1/3, 2/3, Z; 1/3, 2/3, 1/2: 2/3, 1/3, i; 2/3, 1/3, (1/2-z); Chromium 0, 0, 0: 0, 0, 1/2; 2x, 2, 1/4; 232, x, %; X, 22, 1/4; X, 2x, 3/4; x. x, 1/4; x, x, 3/4; The values of x and z were calculated for the alloy mentioned and found as follows: z — 0.061, x = 0.165. The values assumed in the intensity calculations were those for an ideal close-packed lattice or z = 1/16, x = 1/6. Work in the Ti-Mo-Cr system indicates that y2 the hexagonal modification of TiCr2, is the stable phase above 1300°C, while y1 with the cubic structure is stable below 1000°C. X-ray examination of a number of alloys annealed at intermediate temperatures showed that the hexagonal and cubic phases can coexist. Alloys quenched from 1000°C and annealed at 1100" and 1200°C showed small amounts of y2 at the higher temperature. A considerable amount of y, seemed present, however, in cast alloys annealed at 1100°C. It further appears that there is a small but definite solubility range for both phases in the ternary system. Acknowledgment The results of this paper represent work carried out in conjunction with a project sponsored by Watertown Arsenal, Contract No. DA-11-022-ORD-272. References 'M. K. McQuillan: Journal Inst. Metals (1951) 79, p. 379. 2 P. Duwez and J. L. Taylor: Trans. ASM (1952) 44, p. 495. W. J. Van Thyne,. H.. D. Kessler, and M. Hansen: Trans. ASM (1952) 44, p. 974. 1 F. B. Cuff, N. J. Grant, and C. F. Floe: Trans. AIME (1952) 194, p. 848; Journal of Metals (August 1952). Unpublished Research, Armour Research Foundation. "H. J. Wallbaum: Ztsch. Krist. 103, p. 391.

Jan 1, 1954

By F. H. Deily, Jean M. Quets, Milton E. Wadsworth, John R. 222-000-000-012 Lewis, D. S. Rowley, R. J. Howe

Samples of synthetic magnetite were reduced in hydrogen-water vapor atmospheres in the temperature range 450o to 900oC. The reaction was always surface controlled, indicating the final products of reaction are nonfirotective. Three separate cases have been identified from the kinetic results: Case I, reduction of magnetite to iron below 570°C; Case II, reduction of magnetite to iron above 570°C; and Case 111, reduction of magnetite to wustite above 570 oC. In Cases I and 111 the kinetics have been explained by the formation of oxygen anion vacancies in the magnetite surface followed by associated diffusional processes. In Case 11 the observed kinetics have been related to the concentration of iron cation vacancies in the wustite layer formed, followed by associated steady-state diffusional processes. The concentration of cation vacancies in the wustite is maintained constant by the magnetite-wustite equilibrium. THE reduction of the oxides of iron has been a subject of study and interest for many years. However, few attempts have been made to interpret the results in terms of the mechanism of reduction of an iron oxide by either hydrogen or carbon monoxide. Stalhane and Malmberg' using CO, H2, and CO-Hz mixtures, developed the rate expression: where m = mass of oxide reduced, t = time, k = a constant, s = surface area, P = partial pressure of of CO or H,, and P, = partial pressure of the reducing gas at equilibrium. The rate of reaction per unit area was proportional to the difference between the partial pressure of the reducing gas and its pressure at equilibrium. Hansen, Bitsianes, and Joseph2 studied the reduction of pellets of hematite to magnetite with mixtures of CO-CO,. They concluded that below 450°C the reaction proceeded according to a model in which CO reacts with the hematite surface producing an oxygen ion vacancy. The rate controlling step was then assumed to be oxygen ion diffusion through vacancies resulting in the formation of magnetite. They derived an expression giving the rate of reduction proportional to the cO/CO, ratio. Recently McKewan3 published results for the reduction of magnetite spheres in atmospheres below 570°C. He explained his results by an equation of the form where K, is the equilibrium constant for wustite-iron equilibrium attributed to the formation of wustite as an intermediate in the reduction of magnetite. According to McKewan, Kp is an equilibrium constant for H, -HO adsorption in which oxygen is deposited on the surface from the H,Oand subsequently acts as a poison for reduction by hydrogen. Sample Preparation and Experiments. In this work the authors used the same apparatus and experimental procedure employed in the hydrogen reduction of magnetite. Sintered disk samples weighing approximately 1.5 g and measuring 1.2 cm in diameter and 0.25 cm in thickness were prepared by a method described previously.4 Partial pressures of hydrogen and water vapor were controlled by bubbling hydrogen through a series of flasks containing distilled and deionized water maintained at constant temperature in an oil bath. The total flow rate of the reacting gases—hydrogen and water vapor—was approximately 0.5 liter per min. The entire external system was maintained at a temperature above the oil bath to prevent condensation of water vapor. This was accomplished by wrapping electrical resistance elements over all surfaces. The glass column containing the weighing system-a McBain balance suspended from a gold chain-was enclosed in an aluminum tube heated by nichrome resistance wire enclosed in an insulating material. The temperature of the glass column was held constant by means of a series of thermocouples connected in parallel to a Leeds and Northrup temperature controller. This was necessary since variations in temperature resulted in expansion and contraction of the glass column and could be readily observed with the cathetometer. The spring extensions were measured through a window with a gaertner cathe-

Jan 1, 1962

By O. J. C. Runnals

The intermetallic compounds NpAl2, NpAl3, and NpAl have been prepared, and examined by X-ray diffraction methods. The compounds are isostructural with the corresponding U-Al compounds. NpAl3 is face-centered cubic with a = 7.785A and has the MgCu2 structure. NpAl is simple cubic with a = 4.2624 and has the AuCU3 structure. NpAl4 is body-centered orthorhombic with a = 4.428, b = 6.268, and c = 13.71A. The published description for the atomic positions in UAl, applies also to NpAl4 THE U-Al system has been examined by Gordon and Kaufmann.1 They identified the following intermetallic compounds: UAI2, UAl3, and a third, tentatively identified as UAl5. A structure analysis of the latter compound by Borie2 proved that the formula UAl4 was more consistent with the X-ray data. The crystal structures of UAl2 and UA have been reported by Rundle and Wilson.3 UAl2 was found to be isostructural with MgCu. The atomic positions in the simple cubic UA1, cell were found similar to those in the AuCu3 structure. Three analogous compounds exist in the binary system Np-Al. X-ray data for the compounds NpAl2, NpAl3, and NpAl4 are reported below. The neptunium used in the investigation was supplied through the courtesy of the Argonne National Laboratory as neptunium (V) nitrate. It was stated to have a radioactive content of 99.25 pct Np237. The impurity limits had been established by a spectrographic analysis given in Table I. Any titanium, boron, or bismuth impurity should be effectively removed during the fluorination of NpO2 to NpF4, and sodium, lithium, magnesium or strontium during the alloying procedure. The oxalate ignition technique, described by Westrum for the preparation of finely-divided reactive PuO2, was used.The neptunium (V) nitrate solution, containing 100 mg Np, was evaporated to dryness on oxalic acid crystals. The resulting oxalate was calcined to NpO, by heating in platinum at 650°C for 2 hr. An equimolar mixture of anhydrous hydrogen fluoride and purified hydrogen was passed over the NpO2 for 2 hr at 500°C. According to Fried and Davidson" the above fluorination conditions should produce the purple-black fluoride, NpF3 However, the light-green product showed only NpF4 lines on an X-ray diffraction pattern and contained only an estimated 5 pct of finely dispersed black NpF3 particles on microscopic examination. NpAl3: An intimate mixture of 50 mg of neptunium fluoride and aluminum powder (99.99 pct pure, —28 to $60 mesh) was heated to 900°C in a BeO crucible in vacuum by a tungsten coil for 2 hr, to allow the following reaction to proceed: NPF4 + 7Al + NpAl, + 4AlF. [1] The formation and sublimation of aluminum mono-fluoride in this system was verified from an X-ray diffraction analysis of the sublimate. The diffraction pattern was similar to one obtained in the aluminum reduction of UF4 to UF3,6 showing both Al and AlF3 lines. The resulting alloy was sintered at 1100°C for 1 hr. A powdered specimen of the crystalline product was sealed in a thin-walled quartz capillary for X-ray examination. The photograph was taken on a 14.32 cm General Electric powder diffraction camera, using filtered copper radiation. The films were calibrated in terms of a NaCl standard pattern. The wavelengths used in the calculations were 1.5418A for Cu K and 1.5405A for Cu K The powder diffraction pattern showed that NpAl is simple cubic with a = 4.262 % 0.005A, and is isostructural with UA13 where a = 4.27A1 or a =

Jan 1, 1954

By A. U. Seybolt

The solubility limit of oxygen in columbium has been determined in the range between 775' and 1100°C by means of lattice parameter measurements and microscopic examination. The solubility is a function of temperature and varies, in the range given above, from 0.25 to 1.0 pct O, respectively. BECAUSE of the marked deleterious effect of oxygen upon the mechanical properties of some of the transition metals, it is desirable to know something about the solubility of oxygen in these metals. The brittleness caused by oxygen in solution is particularly marked in the case of the group VA elements, vanadium, columbium, and tantalum. The solubility of oxygen in vanadium has already been reported in an earlier paper,' and Wasilewski2 has given a value (0.9 wt pct) for the solid solubility of oxygen in tantalum at 1050°C. Brauer3 in 1941 investigated the Cb-0 system up to Cb2O5, but made no real effort to investigate the extent of oxygen solubility in the metal. He made the observation, however, that this solubility must be less than 4.76 atom pct (0.86 wt pct) oxygen. This estimate was made from X-ray diffraction results on the alloys CbO, CbO, and CbO; all alloys consisted of the terminal (Cb) solid solution plus CbO, but the last alloy containing 4.76 atom pct 0 showed only three very weak CbO lines. It is surprising that Brauer, by examining only three alloys, arrived at an estimate of the solubility which agrees very well with the results to be reported herein. Experimental Procedure A columbium strip obtained from Fansteel Metallurgical Products was cut into strips, 0.020x1/2x2 in. Two holes, about 3/16 in. in diameter, were made near the ends of the strips in order to hold them against a flat steel block for mounting in a General Electric X-ray spectrometer for lattice parameter measurements. The same holes were used to hang the specimens inside a fused silica vacuum furnace tube which was part of a Sieverts' gas absorption apparatus. The apparatus and method of adding oxygen gas has been previously described.1 According to the supplier, the columbium obtained had the analysis given in Table I. After degreasing the samples, approximately 0.001 in. was etched from each side of the samples in order to remove possible surface impurities from the last rolling operation. For this purpose the following cold acid pickle was found satisfactory: 8 parts HNO3, 2 parts H2O2 and 1 part HF. Various Cb-O compositions were obtained up to 0.75 wt pct O by the gas absorption and diffusion technique. After the sample had absorbed all the oxygen gas added at 1000°C, an additional 24 hr was allowed for homogenization. This treatment appeared to be adequate, as shown by the linearity of the lattice parameter-composition plot. More concentrated alloys were prepared by arc melting mixtures of Cb and Cb2O5 since it was very time-consuming to make Cb-0 alloys in the neighborhood of 1 pct O, or over, by the diffusion method. When the flat strip specimens were used, they were ready for the X-ray spectrometer after cooling from the Sieverts' apparatus. The cooling rate obtained by merely allowing the hot fused silica furnace tube to radiate to the atmosphere (when the furnace was lowered) was sufficiently fast to keep the dissolved oxygen in solution. Arc-melted alloys were reduced to —200 mesh powder in a diamond mortar, wrapped in tantalum foil, sealed off in evacuated fused silica tubes, and then heat treated as indicated in Table 11. The fused silica tubes were quickly immersed in cold water without breaking the tubes after the heat treatments. The tantalum foil prevented reaction between the fused silica and the sample; there was no reaction between the powdered samples and the foil at 1000°C, but some trouble was experienced at 1100°C. At this temperature level a reaction between the sample and the foil was sometimes observed, which resulted in erroneous parameter values. Experimental Results Hardness Tests: Since most of the X-ray samples were in the form of flat strip, it was convenient to obtain Vickers hardness numbers as a function of oxygen content. Compared to the V-O case,' oxygen hardens columbium much more slowly, presumably because of the larger octahedral volume in colum-bium (about 12.0 compared to 9.3Å3 in vanadium), hence, requiring less lattice strain for solution. The plot of VHN vs wt pct O is shown in Fig. 1.

Jan 1, 1955

By Bunting S. Crocker

PEBBLE grinding at Lake Shore is not a temporary wartime substitute. The tube milling plant, with a 1000 ton per day capacity, grinds a hard siliceous ore to 90 pct - 325 mesh. The plant, prior to using pebbles, was consuming 4.3 lb of 1 1/4-in. grinding balls per ton of ore, which amounted to 785 tons of balls per year. At September 1951 prices, $132.60 per ton, this steel cost amounted to, $104,400 per year, or $0.285 per ton milled. By the Lake Shore method of substituting screened rock for this steel, all of this cost is saved. This is one of the major economies in Lake Shore mill practice. Regardless of the ultimate price of grinding balls, a change, back to steel balls is not considered. The present pebble plant is more flexible than a steel ball plant and equally efficient. For example, if it is desired to change the size of grinding media, the pebble charge in any mill can be changed completely in 4 to 5 days, as against 76 days to change completely a 1 1/4-in. steel ball charge. To change pebble size it is necessary only to change two sets-of screens and clean out the rock feed storage bin. This will take 8 to 10 days as against 3 to 4 months to clean. out the customary supply of grinding balls kept on hand. Also it has not always been ' possible to purchase all desired sizes of balls at any price. In an analysis of savings effected by the use of the pebble mills, the flexibility of the Lake Shore grinding plant should be discussed, as it has a direct bearing on these savings. The plant has always used several units to handle tonnage rather than sending all the tonnage through a single unit. This principle may result in using small diameter mills, but no objection to that is seen. At no time has any advantage been found in cost per ton ground in large diameter mills. Both the capacity and the power of any mill varies as the diameter raised to the 2.6th power. Consequently large or small mills are equally efficient, and a plant should be designed to use as many units-or combination of units as is consistent with reasonable operating practice. Mills under 5 ft diam are harder to reline, etc. To define the case at Lake Shore, .2600 tons per day formerly were milled in seven 7x6-ft ball mills and twelve 5x16-ft (and two 6x16-ft) tube mills.* This gave an excellent test plant. and an extremely efficient-one. In this plant the ratio of ball mills to tube mills was 1: 2. When the much cheaper pebble mills were substituted for the tube mills, this. ratio -was changed to one ball mill to four pebble mills to take the greatest possible advantage of the cheaper operating mill, i.e., the pebble mill. This flexibility without loss in efficiency has been an important item in the cost savings. It is interesting to note that the use of pebbles for fine grinding was. proved first in the laboratory in a 12-in. ball mill. In fact, since 1934 all testing on -.8 mesh material has been done in this 12-in. mill. Scope of the Tests A paper on fine grinding at Lake Shore Mines was published in July 1940.1 This paper covered 7 years of intensive research on fine grinding as well as sizing methods and equipment, plant scale grinding tests on 5x16-ft tube mills with and without .grate discharges-both with 1 1/4-in. and 3/4-in. balls, the use of laboratory mills to evaluate plant changes, and several reports on classifiers and classification. In the following July the addendum report' was added in which the idea of series-circuit grinding was introduced, and the results of running five stages of tube mills and bowl classifiers were shown. Since 1940, the ball milling end of the plant has been altered extensively as a result of tests on the use of 3 1/2-in. rods in 7x6-ft mills and the use of the Tyler repulping screen with from 7 to 14 mesh screens. These tests are, lengthy and may be covered in a separate 'report later. The scope of this report is confined to ore ground by rod milling and ball milling until it passed through an 8 mesh Tyler Ty-rod screen. The -8 mesh screen undersize then was pumped to a primary bowl classifier in open circuit and the sands .from the bowl sent to the primary pebble mills, see Fig: 1. In the pebble mill circuit the ore is ground to 90 pct -325 mesh (24 pct + 28 microns) In studying the flowsheet, attention should be paid to the efficiency of the classification equipment used. The Tyler repulping screen is an efficient machine on the 8 to 10 mesh separation, and the bowl classifier is equally efficient at the 325 mesh separation. Efficient classification is a necessity for series-circuit stage grinding. The ore is hard siliceous porphyry, 60 pct SiO2, 80 pct insoluble. Its grindability at different. meshes has been shown near the top of 'the list in F. C. Bond's grindability tests' Lake Shore is not shown, but an adjacent-mine with identical ore, Wright-Hargreaves, is. Reasons for the-Changeover Since 1936 grinding balls have been rising steadily in price with no sign of stopping. For a mill that used 4.5 to 5.2 lb of grinding balls for every ton of ore ground this rise represented an alarming increase in grinding costs. In many cases the quality of the grinding balls fell off as the scrap steel became more difficult to obtain. The ratio of tube mills to ball mills increased with the use of the Tyler repulping screen in the ball mill circuit. Originally only 3.0 lb of balls per ton were used in the tube mills, and this

Jan 1, 1952

By R. J. Murphy, N. J. Grant, J. W. Dowding

A large number of blast furnace slag-metal tests were examined to determine if the manganese reduction could be used as a primary indicator of the degree of oxidation or reduction of the slag and of its desulphurizing power. Slag basicity and temperature were also evaluated. Two laboratory heats were made and sampled prior to reaching equilibrium to check blast furnace data. IN a recent investigation of the factors affecting desulphurization in the blast furnace, is was evident that manganese reduction appeared to parallel the course of desulphurization. Grant, Kalling, and Chipman1 pointed this out in a series of time studies utilizing closely controlled laboratory melts. Fig. 1 is a composite plot of sulphur removal and manganese reduction as a function of time under two slags of different basicity. Manganese reduction appears to approach equilibrium at approximately the same rate as does sulphur. It was also demonstrated that the addition of oxygen to the slag, as manganese oxide, caused a sharp reversal of sulphur from the slag to the metal.' It has been shown that "Excess CaO" was a primary factor in measuring the degree of desulphurization under ideal reducing conditions,1,2 the following reaction being representative of the process: CaO (slag) + S + C (solid) = CaS(slag) + CO (gas) It was also evident that a second reaction could drive the sulphur from the slag into the metal. A suggested reaction was' CaS (slag) + 0 = CaO (slag) + S Any change in the oxidizing power of the system would thus affect both the sulphur and the manganese without causing any change in the calculated basicity of the slag. "Excess CaO," "Excess Base," and other similar basicity values, under such oxidizing conditions, would therefore not be the best measure of desulphurizing power; instead, as was shown by and Chipman" he oxygen content of the slag at low oxygen levels would be the controlling factor. Unfortunately, the extent to which FeO is reduced in the blast furnace makes it difficult to utilize slag FeO as an accurate indicator of the degree of oxidation. By comparison, manganese reduction in the blast furnace proceeds more slowly and is generally only about 40 to 70 pct complete. manganese, which is present in significant amounts and is readily analyzed, offers an opportun-

Jan 1, 1954

By R. B. Mears, G. F. Sagar, R. H. Brown

There are well recognized procedures for determining the various tensile, fatigue, and other mechanical properties of the common structural materials. This makes it possible for engineers to design structures of various materials which have adequate initial strength to stand the stresses to which they are subjected in service. There is also considerable general information about protective measures suitable for protecting the usual structural materials from the effects of ordinary environments. However, often insufficient quantitative information is available on the combined effects of stress and corrosion to permit the designer satisfactorily to appraise the structure from the stress-corrosion standpoint. This situation is further complicated by the fact that the stresses causing stress¬corrosion failures are usually not the design stresses but rather the residual forming and assembly stresses which are generally of unknown magnitudes. Thus, tests which will rapidly evaluate the susceptibility of materials to stress-cor¬rosion failures are extremely useful. Of particular value are tests which can be applied to built-up structures as well as to simple specimens, since, as mentioned above, residual stresses often are caused by fabricating procedures and assembly operations. The present paper contains

Jan 1, 1945

By A. E. J. Engel

INDUSTRIAL talcs and ground soapstones both include earth materials of different chemical and mineral compositions. In general, the industrial talcs are composed of silicates that contain appreciable amounts of magnesia. Generally talc, the mineral, is a predominant or at least common constituent. Talc, the mineral, is a hydrous magnesium silicate, with a suggested theoretical formula H2Mg3 (SiO3)4 or H2O.3MgO.4SiO2, which postulates 63.5 pct SiO2, 31.7 pct MgO, and 4.8 pct H20.11 Actually different single grains or leaves of pure talc have variations in water content ranging from 3.5 pct to more than 7 pct, as well as slight differences in the proportions of MgO and Si02.16 Only a very small percentage of the ground industrial talcs produced in the United States approaches the composition given above (see Table 1). The purer talcs invariably occur as alteration products of magnesium carbonate rocks. Some of these relatively pure talcs include compact, massive types largely mined in California, which are designated as steatite.38,58 In general, steatites cannot contain in excess of 1.5 pct CaO, 1.5 pct combined FeO and Fe203, and 4 pct A1203. The less pure varieties of massive talc and mixtures of magnesian silicates are commonly called soapstones, or merely talc. Many industrial earth products classified as talc or as soapstone contain a variety of minerals, especially serpentine (H4Mg,Si2O9), chlorites (hydrous magnesium, iron, aluminum silicates), tremolite (Ca2Mg5H2[SiO3]8), anthophyllite ([MgCa]SiO3), diopside (CaMg[SiO3]2), and quartz (SiO2). The carbonates calcite (CaC03), dolomite (CaMg[CO3]2), and magnesite (MgCO3) are also present in some industrial talcs and soapstones. Some of these minerals, as well as sulphides, sulphates, and iron and manganese oxides, if present at all or in excess of minute amounts, may alter the composition of the industrial talc sufficiently to restrict materially its use or to lower or destroy its value. These factors are discussed in a subsequent section of this chapter.

Jan 1, 1949