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By W. W. Stephens, W. J. Kroll, H. P. Holmes

THE only two methods for producing commercial quantities of malleable zirconium, up to now, have been using magnesium reduction of the anhydrous chloride under a neutral gas, and using purification of raw zirconium by the iodide dissociation method on a hot filament. The purity of the metal obtained by the latter process is about the same as that resulting from the chloride reduction, with the exception of the oxygen content, which may be about 0.05 pct lower in the iodide metal. Even traces of oxygen have a strong hardening effect on zirconium. Since, in the iodide process, the impurities, Si, Al, Fe, Ni, and Mg in the raw zirconium used, are carried over, it would appear uneconomical to use this method of refining solely to eliminate the traces of oxygen, unless very soft metal is desired. One important step to improve the iodide method, namely, dissociating pure iodide made from carbide and recycling the iodine, which would change this refining process into a method for extracting zirconium from the ore, has not yet been made. The Bureau of Mines, by using the chloride reduction, wanted to produce quantities of a reasonably pure and malleable metal at low cost for large-scale industrial use. This aim has been achieved, and a pilot plant permitting production of 600 lb of malleable zirconium per week will be described (fig. 1). Briefly, the Bureau of Mines process consists of reducing purified gaseous anhydrous zirconium chloride with fused magnesium under a noble-gas atmosphere. The reaction product, magnesium chloride, and any excess magnesium metal present are removed from the sponge zirconium in the next step by fusion and evaporation in a good vacuum at about 925°C. In this process, care is taken to keep air out of contact with the hot metal, which otherwise would contaminate the product with oxygen and nitrogen. Both these impurities embrittle zirconium even when present in an amount as low as 0.1 pct. A number of previous reports1-3 describe the method and the various improvements that finally led to a workable process. The major steps made were the production of large quantities of carbide, which is the raw material for producing the chloride, its chlorination with reasonable efficiencies, and the elimination of iron trichloride contained in the raw chloride, as well as that of the zirconium oxide which is always present in this product. The physical nature of the anhydrous chloride, which sublimes at 331°C at atmospheric pressure and melts at 420°C under a pressure of 25 atm, made it necessary to provide a special safety device on the purification and reduction vessels in the form of a lead-alloy seal, permitting escape of excess gases if pressure tended to build up. The main difficulties encountered in the reduction and in the following step, salt separation in a vacuum at elevated temperature, were caused by the material from which the reaction pot was constructed—iron. This metal reacts with zirconium at about 940°C with formation of a eutectic. The last step, salt separation by evaporation of the magnesium and magnesium chloride in a vacuum, is quite unconventional and has not been used before on such a scale. It is only due to the improved construction of high-vacuum pumps, especially oil-diffusion pumps, that such a method could be used. The various steps of the Bureau of Mines process, as described in the general outline above, may be summarized as follows: (1) production of the carbide, (2) chlorination of the carbide, (3) purification of the raw chloride, (4) reduction of the pure chloride with fused magnesium, (5) separation of excess magnesium and magnesium chloride in vacuum at elevated temperature, and (6) melting of the sponge obtained. Production of Carbide The arc furnace, described in a previous report,' was improved both to reduce the graphite consumption caused by the burning of the bottom plates and to concentrate the heat in order to obtain better power efficiency. This was achieved by providing the bottom with graphite plates entirely embedded in refractory bricks, the contact with the current being made with three water-cooled copper plugs. Figs. 2 and 3 show the arrangement. The crucible, made

Jan 1, 1951

Jan 1, 1934

Jan 1, 1951

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Jan 1, 1938

Jan 1, 1893

By E. Cortese

PHOSPHATE occurs in many places in Egypt,. in two main zones: one in Upper Egypt, along the Nile Valley, principally on the right side, and one near the Red Sea coast. In the Nile zone, the principal layers of phosphate rock are to be found: in the mountains east of Mahamid (right side of the valley); in the hills near Sibaiya, also called Sebaieh (both sides); in the hills of Agula, Hagaza and Gurn (right side); and further on, along the cancel road leading from Kena to Kosseir, a few miles east of Legheita's Oasis. Following, that track, after, having crossed the watershed, underlain by rocks like granite, serpentine, porphyry and diabase, one comes again to the Cretaceous formation containing considerable quantities of phosphate, at Gebel Duwi, Gebel Nakheil and Gebel Kosseir El Kadim, not far from the coast. More to the north, in the hills near Safaga Bay (Um El Uettat El Wasif) is another rich bed of the same formation. There are reports of phosphate existing near Suez and in the Sinai peninsula, and possibly some other zones can be traced or discovered in the future. The mines are well developed on the right bank of the Nile at Sharawna (near Sebaieh Station) and along the Red Sea coast, at' Safaga and near Kosseir. Prospecting work has been done at Gebel Duwi, Gebel Gurn, Agula, Hagaza, and near Mahamid. The phosphatic formation in Egypt is quite variable, not only from place to place, but even within small areas. The phosphate is all of Cretaceous age, as is proved by the fossils found in it. It is considered to belong to the Campanian or, more appropriately, to the Maestrichtian series. The principal fossils are: Alectryonia Villei Coq. sp.; Roudereia Auressensis Coq. sp.- R. Drui Mun. Chalm.; Trigonoarca multidentata, Newton.; Cardita libyca, Zittel; Libycoceras Ismäely, Zittel; Nautilus sp.; Ancystrodon libycum Dam.; Corax pristodontus Ag.; Lamma biauriculata Zittel sp. Above the Maestrichtian beds, we have the Danian series, unconformably covered by Lower Eocene beds. Under the phosphate is a grayish marly clay, and beneath this, bluish-gray scaly shales resting on the Nubian sandstone (Santonian).

Jan 2, 1918

By John Birkinbine

A specimen of brown hematite, taken from an iron-ore mine near Anniston, Alabama, exhibits a metallic streak or thread running throngh it. This specimen having been sent to me, I have no personal knowledge of its occurrence; but Mr. Albert E. Noble

Jan 1, 1895

Jan 1, 1932

By Russell A. Carter

Seven years of rising silver prices have effectively revived an historic Idaho mining district and given it a new lease on life. Initial production earlier last year from the DeLamar open-pit silver mine in southwestern Idaho ushered in a new era of mineral production in a region that has weathered boom-and-bust cycles reaching back the better part of a century.

Jan 1, 1978

Executive. CHARLES F. RAND, Chairman. JAMES F. KEMP, JOSEPH W. RICHARDS, ALBERT R. LEDOUX, BENJAMIN B. THAYER. Membership. BENJAMIN B. THAYER, Chairman. WALTER R. INGALLS, JOHN H. JANE WAY, JR., JOHN D. IRVING, HERMAN A. PROSSER. Finance. EDWARD L. YOUNG, Chairman. KARL EILERS, JAMES GAYLEY.

Jan 4, 1913

Jan 1, 1949

By Charles P. Williams

THE successful production of zinc white or oxide on a commercial scale in this country dates from the issue of the patent of Samuel Wetherill, for the preparation of the material (November, 1855), and

Jan 1, 1877

By Charles P. Williams

The successful production of zinc white or oxide on a commercial scale in this country dates from the issue of the patent of Samuel Wetherill, for the preparation of the material (November, 1855), and

Executive.. CHARLES F. RAND, Chairman. JAMES F. KEMP, JOSEPH W. RICHARDS. ALBERT R. LEDOUX, BENJAMIN B. THAYER. Membership. BENJAMIN B. THAYER, Chairman. WALTER R. INGALLS, JOHN H. JANEWAY, Jr., JOHN D. IRVING, HERMAN A. PROSSER. Finance. EDWARD L, YOUNG, Chairman. KARL EILERS, JAMES GAYLEY. Library. JAMES F. KEMP, Chairman. JOHN HAYS HAMMOND,3 E. GYBBON SPILSBURY,2 ALES. C. HUMPHREYS 4 BRADLEY STOUGHTON.

Jan 7, 1913

By Roy C. Kirkman

It is with great pleasure that I read Mr. Howard M. Wells article in the December 1978 issue of MINING ENGINEERING entitled: "Optimization of Mining Engineering Design in Mineral Valuation." Mr. Wells very adequately presents the case and point that there are a great number of variables which must be analyzed during an economic evaluation of an FUND RESOURCE, such as copper or uranium.

Jan 4, 1979

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Jan 1, 1938

Oct. 8-13, 1917 COMMITTEE ON ARRANGEMENTS H. A. BUEHLER, Chairman, W. E. McCOURT, Secretary, C. J. ADAMI, Southeastern, J. A. CASELTON, Entertainment, F. W. DEWOLF, Book, , E. F. GOLTRA, Finance, L. L. HUTCHISON, Tulsa, E. McAULIFFE, Transportation, P. N. MOORS, Reception, MRS. P. N. MOORE, Ladies, J. D. ROBERTSON, Publicity, VICTOR RAKOWSKI, Joplin., H. A. WHEELER, Excursions, A. THACHER.

Jan 7, 1917

The following Nominating Committee having been already appointed and approved by the Executive Committee in accordance with authority vested in the Executive Committee by the Board of Directors, was approved by the Directors: John V. N. Dorr, Chairman, Percy G. Beckett, J. W. Hutchinson, Julian Kennedy, William H. Linney, Charles W. Merrill, and E. Gybbon Spilsbury. The question of the purchase of Liberty Bonds, as well as that of bringing to the attention of the members the advisability of the purchase of these bonds, was referred to the Finance Committee. Sixty Members, four Associates, and thirty-six Junior Members were elected. Two Members were reinstated. Eight resignations were accepted.

Jan 7, 1917

By Bunting S. Crocker

EBBLE grinding at Lake Shore is not a temporary BlE 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 11/4-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-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.' 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-in. and -in. balls, the use of laboratory mills to evaluate plant changes, and several reports on classifiers and classification. In the following July the addendum report2 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-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 SiO,, 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, 1953

By Bunting S. Crocker

EBBLE grinding at Lake Shore is not a temporary BlE 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 11/4-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-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.' 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-in. and -in. balls, the use of laboratory mills to evaluate plant changes, and several reports on classifiers and classification. In the following July the addendum report2 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-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 SiO,, 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, 1953