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By E. A. von Hahn, T. R. lngraham

Cementation rates ulere studied by rotating an elec-tropolished or etched copper strip in aqueous solutions, of either perchloric acid or alkaline cyanide, containing silver ions. The rates of cementation were more rapid in acidic media than in cyanide media. In both, the rates varied with the rate of rotation of the copper strip. The deposits formed in the acidic solutions were finely divided, loosely adhering powders. Those formed in the cyanide solutions were dense and adherent. The presence of the deposits influenced the cementation rates. In the acidic solutions the rate was enhanced, possibly because of the increased cathodic area. In the alkaline solutions the rates were decreased in the presence of the deposits. This has been attributed to restricting the diffusion of the copper ion from the rnetal outward into the bulk of the solution. In an earlier paper1 the authors described a kinetic study of the cementation of palladium on copper in perchloric acid solutions. That work indicated that there were two stages in the palladium cementation process. The first, more rapid stage was consistent with rate control by the diffusion of Pd11 ions to the copper surface and/or by chemical reaction at the surface. The second stage was consistent with rate control by the diffusion of copper ions from the copper surface, through the deposit, out into the main body of solution. The effect of the type of deposit on the rate of cementation is of particular interest because it may be one of the primary features involved when large quantities of metal are to be cemented from solution. No substantial investigations of the effect seem to have been made. Accordingly, an extension of the previous work was arranged to study the cementation of silver on copper. This system was selected because of the convenience of the analytical methods, the previously established technology with copper, and the fact that the system could be studied in both acidic and alkaline media. By selecting perchloric acid and alkaline cyanide solutions as the media, it was hoped that some assessment might be made of the effects, on cementation, of having the silver ion present in a virtually uncomplexed state and in a highly complexed state. EXPERIMENTAL The cementation rates were studied, as previously described,' by rotating a copper strip (1.0 by 23.2 cm) clamped to the peripheral surface of a lucite cylinder. The solutions were kept at constant temperatures (±0.05°C) under an atmosphere of purified nitrogen, and samples were taken periodically for analysis. The initial solution volume was 1000 ml and the sample volume 5 ml. The initial silver(1) ion concentrations were made low (0.5 to 1.0 x 10-4 moles per liter) to minimize the influence of the cemented deposit on rates. The solutions were prepared by dilution of suitable aliquots of silver perchlorate and silver cyanide stock solutions. Both stock solutions were prepared from purified silver powder (Johnson, Matthey, and Mallory Ltd.) with redistilled deoxygenated water, and they were kept under an atmosphere of purified nitrogen. To prepare the stock solutions, weighed amounts of silver powder were dissolved with nitric acid. For the AgC104 stock solution the silver nitrate solution was evaporated twice to near dryness with perchloric acid and then made up to volume: For the NaAg(cN)2 stock solution, the silver ions were precipitated with sodium hydroxide solution. The precipitate was filtered, washed thoroughly with redistilled water, dissolved with 1.1 times the required stoichiometric amount of sodium cyanide solution, and made up to volume. The small amounts of free perchloric acid and sodium cyanide present in the stock solutions were disregarded in the preparation of the solutions. The copper strips were cut accurately from 0.025-in. sheet (American Metal Climax OFHC brand) and annealed for 1.5 hr at 470°C in a stream of nitrogen. Analyses of the solution samples for silver and copper were done with a Techtron Model AA-3 atomic absorption spectrophotometer. Calibration standards of the same composition as the experimental solutions were prepared and analyzed simultaneously with the samples. No difficulty was experienced in the analyses, and the reproducibility was within 1 to 2 pct in both alkaline cyanide and perchloric acid solutions.

Jan 1, 1968

By Paul W. Zimmer, Carl E. Dutton

Iron ore in the Menominee district is mined from two iron-formations of middle Precambrian age. The older formation is present in the northeastern part; is composed mainly of hematite, magnetite, quartz, and minor silicates; and contains about 34 per cent iron. The rock has been so coarsened by meta- morphism that concentration of magnetite and hematite is feasib!e, and pellets containing more than 60 per cent iron are being produced. The older formation is also present in the southeastern part where it has 1:een only slightly metamorphosed. Ore containing more than 50 per cent iron was formerly mined from local residual concentrations of iron oxides from which silica had been sufficiently leached, or replaced by iron oxide, or affected by combinations of these processes. The younger iron-formation occurs in the western part of the district and, if unaltered, is interlayered siderite and chert. The ore in this area also contains more than 50 per cent iron and formed as local residual concentrations but in two stages. The siderite was converted to iron oxides (hematite and "limonite"), and silica was contemporaneously or subsequently removed by leaching, or replacement, or combinations of these processes.

Jan 1, 1968

By C. W. Davis

THE name fuller's earth, which was derived from its early use in "fulling" or removing grease from woolen goods, is a term that is generally considered to designate mineral matter, containing hydrous aluminum silicates of the clay group, which has a high capacity for removing colors from oils, whether of animal, vegetable, or mineral origin. Fuller's earths are usually dried and may be "tempered" by heating or may be treated with water or reagents to improve their efficiency. For our purpose the term "acid-treated earths" will include those products from the partial decomposition of mineral water by acid which are equal to or more efficient than an untreated fuller's earth from Quincy, Fla., when used in bleaching mineral oil by the "contact" process. In general, the contact process for treating oils consists of heating and agitating a mixture of oil and finely divided adsorbent, the latter being subsequently removed by filtration. The term "adsorbent" is used because, although there has been a great deal of controversy over the mechanism of removal of impurities from oils by mineral matter, there is no doubt that adsorption, which involves the surface of the solid, plays a major part.1 The properties that make fuller's earth useful in the treatment of petroleum products by "percolation" and in the purification of edible oils by the contact process have long been studied, but the comparatively recent adaptation of the contact process to the bleaching of petroleum products has made desirable the further investigation of fuller's earth and other adsorbent earths.

Jan 1, 1929

By R. R. Boucher, O. J. C. Runnalls

A pronounced thermal effect has been observed on heating or cooling a1wninum-rich Al-U and Al-Pu alloys. From microscopic and X-ray diffractionstudies, the effectl has been attributed to trnsfor)nations in the inlemetallic phases UAl, and PuAl , involuing rearrangement or cluslering of vacancies The transformation obsrved in Al-20 wi oct U alloys occurred near the a Al-UAl4 eutectic tem-perature of 646°C making it difjicult to detect from heating curves. When cooling, howeoer, thermal mad X-ray analyses indicnted that the high-temperati~re phase labeled p UAL, precipitated initially during euitectic solidification. As solidification continued and after an induction period o-f 5 lo 20 tnin the nu-cleatiorz and growth of the low- twmperature phase, a UAl4 produced an euolution of energy which raised the observed alloy temperature by 1° to 2°C. in Al-Pu alloys the transformation occurred at 645°C, 5 deg below the eutectic solidification temperccture. The eslimated latent heat of transformation was 25 +5 cnl per g PuAl,. The high-tetnpevcl-ture forms of UAl, and PuAl, were easily 9-etccined by chill casting Al-U and Al-Pu alloys and on reheating the alloys the trcltzsforrnation to the a phase was sluggish even above 600°C. Separated single cryslals o-f UAl4, joy example, showed no evidence Of transformalion after heating for 16 hr at 620°C. The transformation rates increased yapidly enough with increasing temperature, however, that a a spontaneous liberation of energy lens observed on occasion when bealing cast Al-20 wt pet U to neal- the RECENT phase studies on A1-Pu alloys have indicated that earlier reported equilibrium diagrams should be modified to take account of several poly- morphic transformations in the intermetallic compound PuAl,.' During the course of the latter work an unexpected heat evolution was observed while cooling a solid alloy consisting of a mixture of a aluminum and PuA1,. The evolution occurred at 645°C, y below the a A1-Pu A1, eutectic solidification temperature. Subsequent thermal-analysis experiments with A1-U alloys showed that heat was evolved there also at a temperature nearly coincident with the a A1-UA1, eutectic solidification temperature of 646°. A search of the literature revealed that similar thermal effects had been observed before for both A1-U and A1-Pu but had never been fully explained.2,3 The purpose of the present paper is to describe thermal-analysis and X-ray diffraction experiments which have led to the conclusion that the thermal effects are due to transformations which involve the rearrangement of vacancies in the intermetallic compounds UA1, and PuA1,. EXPERIMENTAL PROCEDURE The A1-U alloys were prepared by heating super-pure aluminum (99.99 pct +) obtained from the Aluminum Co. of Canada in a graphite crucible surrounded by an induction coil. At 1000°C high-purity uranium metal produced by the Eldorado Mining and Refining Co., Ltd. was dropped into the liquid aluminum and was dissolved completely within 15 min. The impurities in the uranium were A1—4 ppm, Ca-4, C-70, Cr-3, Cu-6, Fe-30, Mg-2, Mn-10, Ni-25, Si-25, and Zn-2. The A1-Pu alloys were prepared by reacting plutonium dioxide with liquid aluminum under cryolite (3 NaF . AlF,) for 10 min at 1100°C in graphite crucibles exposed to the air. The plutonium was 99.8 pct pure, containing trace impurities of Ca, Cu, Fe, Pb, Si, and Zn. The liquid alloys were usually poured into water-cooled molds to provide castings of uniform composition from which samples could be cut for heat treatment and thermal-analysis experiments.

Jan 1, 1965

By K. G. Davis, P. Fryzuk

A study has been made of the effect of undercooling on the grain structure and solute distribution in small ingots of pure bismuth and of a 100 ppm Ag in bismuth alloy. Autoradiographic evidence shows that in undercooled melts a network of dendrites is formed throughout the melt immediately after nu-cleation. At large undercoolings the dendrites are very thin and closely spaced. The origin of the observed grain morphology can be explained on the basis of information about the mode of solidification revealed by the impurity substructure. WHILE a great number of studies of nucleation in undercooled molten metals have been made, comparatively little attention has been given to the mode of solidification from melts with large undercool- ings. Colligan and Bayles1 and Walker2 have measured the rate of advance of the solid-liquid interface in undercooled nickel melts, but the morphology of the solidifying material remained a matter of speculation. Fehling and Scheil3 have described the grain structure in ingots formed from undercooled melts of nickel, palladium, and copper, and a series of Ni-Cu and Ni-Pd alloys. At small undercoolings, equiaxed structures are observed, the grain diameter tending to increase as the temperature of nucleation is lowered. At greater undercoolings, a columnar structure is developed, while with still further undercooling there is a smaller grain size incorporating rather coarse subgrains. All-bright and Colligan4 examined the grain structure shown by ingots solidified from melts of nickel and of Ni-Ag alloy at an undercooling of 105°C, and concluded that considerable grain growth had taken place after solidification. The object of the present work is to correlate the mode of solidification from undercooled melts with both the grain structure and impurity segregation, using tracers to examine the latter.

Jan 1, 1965

By HOWARND N. EAVENSON

THE year 1930 resembled the preceding one in the coal industry in continuing the era of falling prices and 'of the abandonment of unprofitable mines. Practically all coal prices fell, and in the steam sizes during the last half of the year this was particularly true, due to the small industrial demand. No new mines of any size were opened in the bituminous coal industry, but there was a steady increase in the number of cleaning plants of all kinds built in all fields. It is estimated that at least nine million tons per year were added to the previous total of washed coal. The largest washing plant started during the year was that of the Buckeye Coal Co., at Nemacolin, Pa., with a capacity of 650 tons per hour. Fig. 1 shows - the mixing-bin, conveyor galleries, washing-plant and skip hoist, and Fig. 2 the 120-ft. Dorr thickener for collecting the 48-mesh material from the wash water. Dryers are used for drying the steam coal product. The following statement by J. R. Campbell shows the effect of cleaning on Pittsburgh coal in Greene County: "With the advent of the 650-t.p.h. efficient washing plant in Greene County at the Nemacolin mine of the Buckeye Coal Co., it has undoubtedly been demonstrated that the potential coking-metallurgical coals of the county can be brought within the pale of the highest grade high-volatile coals for steel manufacture. A few months' operation indicates that 9% per cent ash in the raw coal can be easily reduced to under 7 per cent ash in the washed coal and the sulfur from 1.60 per cent in the run of mine to 1.20 per cent sulfur in the washed coal.

Jan 1, 1931

By Elwin L. Fisk

The Cordero mine is located in the Nevada portion of the Opalite Mining district that straddles the Oregon-Nevada state boundary. The mercury deposits of the district occur along the margins of the broad east-west graben valley of McDermitt Creek. The only other major producers, the Opalite and Bretz mines, on the northern margin of the graben have thus far exploited only shallow deposits within 100 feet of the surface. Through December 1965, Cordero has produced 94,680 flasks of mercury, the most of which came from the large underground cinnabar deposit. Nearly all of the mercury ore deposits in this district have been found in Miocene rhyolitic intrusives, flows, tuffs, and lake beds. These rhyolites have been argillically altered at depth and extensively silicified at or near the surface. These silicified areas or "opalite" masses were the original cinnabar-bearing outcrops.

Jan 1, 1968

By E. R. Johnson

THE copper concentrator of the Braden Copper Co. is at Sewell, Chile, on the western flank of the main Cordillera of the Andes, at an air distance of approximately 50 miles southeast of Santiago, the capital of Chile. The region is mountainous and space is at a premium because of the rough terrain and the danger of snowslides. The ore, a porphyry copper, is mined by a block-caving method in the El Teniente mine. It is hauled to the crushing plant, a distance of 2.6 miles, through a tunnel because of the severe climatic conditions. The usual large, coarsely set, primary reduction machines found in many ore-treating plants are not required because of the mining method employed and the limiting 12-in. spacing of the grizzlies at the head of each ore pass in the mine. It is the purpose of this paper to describe the numerous improvements made in the crushing section of this large flotation concentrator during the past 15 years to increase the efficiency of the plant and to raise the daily output from around 20,000 to 30,000 tons. The reader should keep in mind that all changes were made within the existing building because of the limited space and the high cost of the heavy mill construction required to withstand the snow loads. The present plant, as well as the former, operates on a 24-hr, 7 days a week basis. FORMER PLANT The crushing plant commenced operations at its present site in 1921, the main equipment being No. 7 1/2 gyratories, followed by 48-in. horizontal Symons disk crushers. Fines were removed by 1-in. stationary grizzlies ahead of each unit. In 1924 a third stage of crushing was provided by the addition of 55 1/2-in. rolls in open circuit. During 1925, the Symons disks were replaced by 73 1/2-in. rolls. All the rolls were changed to closed circuit, with elevators and screens to give a final product of 9 pct plus 3-mesh. The flowsheet of a typical crushing section of this period is shown in Fig I. The ore was withdrawn from a common bin serving the five crushing sections in the plant by means of any number up to six 36-in. wide-apron feeders, which discharged onto a common conveyor belt. This conveyor was equipped with a magnetic head pulley and the crusher attendant was stationed near the discharge end to pick out pieces of mine timber that might be in the ore. The ore was discharged over a 1 3/4-in. spaced bar grizzly and the oversize of this grizzly was crushed by a No. 7 1/2 McCully gyratory crusher set at 1 3/4-in. opening on the closed side. The grizzly undersize joined the gyratory discharge and was conveyed to a set of 73 1/2 by 20-in. Garfield rolls set at I in. These rolls operated in closed circuit with a bucket elevator and two vibrating screens placed in parallel.

Jan 1, 1947

By E. L. Kinsella, F. S. White

Solids fluidization utilized in two ways for the commercial production of lime is described. Crushed —6 mesh limestone is dried and dedusted in a single bed reactor, then calcined in a 5-stage reactor. Construction, operation, and results obtained with both processes are given. THE solids fluidization process brought out by the Standard Oil Development Co. in the early forties for catalytic cracking of petroleum enabled rapid transfer of large quantities of heat from gases to solids under closely controlled temperature conditions. As the technique developed, it was natural that applications for the process outside the petroleum industry would be sought. The calcination of limestone to quicklime requires the transfer of a large quantity of heat at high and closely controlled temperatures. For these reasons, this possible application was one of the first to be investigated. Laboratory work conducted by the Dorr Co. indicated that lime produced by solids fluidization would be of exceptional quality. Calculation of theoretical heat balances showed that savings in fuel could be expected. Accordingly, a pilot plant of 10 tons per day capacity was erected by the New England Lime Co. at Adams, Mass., to substantiate the process. Operation of the pilot plant, previously described,' showed that excellent lime could be produced with a saving in fuel. The work also indicated the necessity of preparing feed to remove the finer fractions if dust losses were to be held to a tolerable level. A single-stage fluidized solids drier-stripper was developed to accomplish this sizing.' Subsequently a commercial lime reactor was erected at Adams, beginning operation in June 1949, followed by air sizer facilities completed in November 1951. This paper will describe these two applications of solids fluidization. The raw material for preparation of lime by the fluidizing process is a high calcium crystalline lime- stone having the approximate chemical composition shown in Table I. The stone is first prepared by crushing and grinding in conventional equipment to pass a 6-mesh sieve. After crushing, the material is sent to the FluoDry unit for drying and dedusting. Fluidized Drying and Sizing As shown in Fig. 1, the FluoDry unit consists of a -in. cylindrical steel shell, 9-ft ID by 22-ft 6-in. overall height. Attached horizontallv at the bottom is a 6-ft diam combustion chamber, approximately 7 ft 6 in. long. A refractory constriction dome, consisting of first-quality fire brick shapes, partitions the inside into two sections. The lower section is called the windbox and the upper the bed compartment. The vertical wall of the shell is lined with 6-in. first-quality rotary kiln blocks. In the bottom of the windbox a hoppered section is formed with castable refractory to permit the windbox to be readily cleaned via a 6-in. screw conveyor. The combustion chamber is similarly lined with refractory shapes. On the 6-in. diam section, 4 in. of insulating brick, HW-26, are used. The inner combustion chamber is lined with 4-in. Korundal brick to withstand the high flame temperatures encountered. An 8-in. steel feed pipe, entering vertically through the top and fitted with an air-operated cone valve,

Jan 1, 1953

By F. S. White, E. L. Kinsella

Solids fluidization utilized in two ways for the commercial production of lime is described. Crushed —6 mesh limestone is dried and dedusted in a single bed reactor, then calcined in a 5-stage reactor. Construction, operation, and results obtained with both processes are given. THE solids fluidization process brought out by the Standard Oil Development Co. in the early forties for catalytic cracking of petroleum enabled rapid transfer of large quantities of heat from gases to solids under closely controlled temperature conditions. As the technique developed, it was natural that applications for the process outside the petroleum industry would be sought. The calcination of limestone to quicklime requires the transfer of a large quantity of heat at high and closely controlled temperatures. For these reasons, this possible application was one of the first to be investigated. Laboratory work conducted by the Dorr Co. indicated that lime produced by solids fluidization would be of exceptional quality. Calculation of theoretical heat balances showed that savings in fuel could be expected. Accordingly, a pilot plant of 10 tons per day capacity was erected by the New England Lime Co. at Adams, Mass., to substantiate the process. Operation of the pilot plant, previously described,' showed that excellent lime could be produced with a saving in fuel. The work also indicated the necessity of preparing feed to remove the finer fractions if dust losses were to be held to a tolerable level. A single-stage fluidized solids drier-stripper was developed to accomplish this sizing.' Subsequently a commercial lime reactor was erected at Adams, beginning operation in June 1949, followed by air sizer facilities completed in November 1951. This paper will describe these two applications of solids fluidization. The raw material for preparation of lime by the fluidizing process is a high calcium crystalline lime- stone having the approximate chemical composition shown in Table I. The stone is first prepared by crushing and grinding in conventional equipment to pass a 6-mesh sieve. After crushing, the material is sent to the FluoDry unit for drying and dedusting. Fluidized Drying and Sizing As shown in Fig. 1, the FluoDry unit consists of a -in. cylindrical steel shell, 9-ft ID by 22-ft 6-in. overall height. Attached horizontallv at the bottom is a 6-ft diam combustion chamber, approximately 7 ft 6 in. long. A refractory constriction dome, consisting of first-quality fire brick shapes, partitions the inside into two sections. The lower section is called the windbox and the upper the bed compartment. The vertical wall of the shell is lined with 6-in. first-quality rotary kiln blocks. In the bottom of the windbox a hoppered section is formed with castable refractory to permit the windbox to be readily cleaned via a 6-in. screw conveyor. The combustion chamber is similarly lined with refractory shapes. On the 6-in. diam section, 4 in. of insulating brick, HW-26, are used. The inner combustion chamber is lined with 4-in. Korundal brick to withstand the high flame temperatures encountered. An 8-in. steel feed pipe, entering vertically through the top and fitted with an air-operated cone valve,

Jan 1, 1953

Mining Methods LUCIEN EATON, Chairman GERALD F. SHERMAN, Vice-chairman CHARLES W. WRIGHT, Secretary Alluvial Mining CLINTON BERNARD CHARLES H. MUNRO CHARLES JANE N H. R. NORSWORTHY Open-cut Mining Iron MAX H. BARBER J. A. MacKILLICAN Copper MICHAEL CURLEY H. B. TEMPEST Underground Mining Iron C. H. BAXTER CARL BREWER TENNEY C. DESOLLAR Copper W. B. DALY A. H. WOHLRAB R. W. THOMAS

Jan 1, 1934

Jan 1, 1901

By Thomas R. Stauffer

The principle that conventional schemes for taxing petroleum or mineral resources are "inefficient" is illustrated using simulation calculations tested against an "ideal" system. Inefficiency is defined as the relative success in maximizing expected government revenues from the resources. Most systems fail because: 1) they leave oil in limbo, i.e. unproduced because of excessive fiscal burden; or 2) they unnecessarily increase the variance in the explorationist'c, rate of return by undertaxing large fields and overtaxing smaller but infra-marginal fields. This increases his discount rate and reduces taxable surplus. An "ideal" tax system is specified which maximizes government revenues while minimizing risk to the operator. Two criteria are developed: 1) the tax falls to zero on fields which yield only the minimum necessary rate of return ("marginal" fields); and 2) the after-tax present value of all fields is the same for all fields above a threshhold size. In particular, marginal fields, while contrib- uting little to expected values, do contribute to reducing variance and hence risk praemia by distributing the exploration costs over a higher probability of successful outcomes.

Jan 1, 1982

By W. M. Albrecht, W. D. Klopp, R. I. Jaffee, B. G. Koehl

Kinetic studies were made of the reactions of tantalum with oxygen, nitrogen, and air at 400o to 1500°C. The tantalum-oxygen reaction is linear from 500° to 1250°C. The tantalum-nitrogen reaction follows a cubic rate law at 400° to 700°C and a parabolic rate law at 800" to 1475°C. The reaction behavior in air is initially parabolic followed by a transition to linear behavior. In the search for high-temperature materials, considerable interest is being shown in the refractory metal, tantalum. It is the third highest melting metal with a melting point of 2996°C. Also, tantalum has excellent ductility, making it one of the most workable refractory metals. In considering high-temperature applications of tantalum, the oxidation kinetics of the metal must be known. Such information also serves as a basis for the development of corrosion resistant tantalum-base alloys. Therefore, this study was made to investigate the reaction of tantalum with air, nitrogen, and oxygen. LITERATURE Several oxides of tantalum have been reported. The pentoxide, Taz05, is the only oxide of tantalum whose identity has been established. A high-temperature modification, aTa2Os, has been reported by several investigators.1-4 A low-temperature phase, ßTa2O5, undergoes an allotropic transformation at 1320o to 1350oC. 5-8 Four other oxides of tantalum have been reported. The oxides TaO2, TaO, and Ta4O have been reported by schonberg.9 A suboxide Ta2O, was observed by Wasilewski 6. However, the presence of oxides lower than Ta2O5 is questioned by Lagergren and Magneli.7 In oxidation studies, vermilyeal0 and Peterson, et al.,12 reported one possible phase intermediate between Ta and Ta2O5. Only Ta2O5 was formed in the tantalum air reaction, as reported by Michae1.l3 Several studies have been made on the kinetics of the tantalum-oxygen reaction. vermilyeal4 investigated the range 50° to 300°C and found that the rate of growth of a thin adherent oxide film could be described by the Cabrera-Mott theory. Gulbransen and Andrew15,18 studied the reaction kinetics of tantalum in oxygen pressure of 1/10 atm at 250° to 450°C. At all temperatures the reaction followed the parabolic rate law for periods up to two hours. The oxidation behavior in the range 500" to 1000°C was found to be linear at oxygen pressures of 0.2 to 600 psi according to Peterson. et al.l1 At very low pressures (1 x 10-3 to 2 X lo-' mm of Hg) Gebhardt and seghezzi17 reported linear oxidation at 800° to 1500°C. The reaction of tantalum with air is similar to the reaction with oxygen. Studies have been made by Waber, et a1.,12 and Michae1.l3 Two nitrides of tantalum, TaN and Ta2N are known. Their structures have been determined by Brauer and Zapp 18,19 The tantalum-nitrogen reaction kinetics have been investigated by Gulbransen and Andrews. 15, 16 The reaction follows the parabolic rate law at 500° to 850°C at a nitrogen pressure of 1/10 ,atm. At the same temperature, the tantalum-nitrogen reaction is much slower than the tantalum-oxygen reaction. EXPERIMENTAL TECHNIQUES Material— The material used in this study was high-purity, electron-beam-melted tantalum obtained from the Temescal Metallurgical Corp. The hardness of the as received ingot was 76 Vhn. The analysis of the material is given in Table I. Methods—Cylindrical specimens of tantalum approximately 0.9 cm in diam and 0.5 cm in length

Jan 1, 1962

By L. W. Rowe, S. S. Cole

A laboratory bench scale unit is described whereby finely divided chlorinatable residues are held for a short period by a restraining bed of a coarse-grained ore of comparable composition to permit 'flash' chlorination of the high surface area powder. Results on chlorinating a finely divicled titania residue using rutile sand as the restraining bed showed that 92 pct utilization of chlorine and equivalent conversion of TiO2 in the fine residue to Ticl4 were attained with a dust loss of about 3 to 4 pct and an equivalent amount of ch1om'nation of the titanium values in the restraining bed. THE chlorination of coarse grain titaniferous ores; i.e., 20 to 150 mesh sizes in fluidized beds is practiced commercially.' One effective method found for the chlorination of a very fine material in a fluidized bed is the "flash" chlorination technique.' By charging the finely divided charge material into the bottom of an established bed of optimum sized rutile, ilmenite, titanium beneficiate, or even an inert material such as sand, chlorination occurs before the dust can pass through the bed. The major requirement is that the bed be less chlorinatable than the charge. In this process, the charge consists of a finely divided (between one and 50 µ) titania residue obtained from a titaniferous ore beneficiation process. The charge is blended with a 20 pct wt basis addition of 20 to 60 .mesh size low volatile coke (to minimize hydrogen chloride formation) and fed to the bottom of the bed with the chlorine gas stream. A ball check device is used to permit entry of the charge and prevent the bed from discharging when the gas flow is cut off. The coarse pieces of coke serve to reduce compaction in the charge mixture and permit sat]sfactory feeding without plugging or jamming. Feed and gas rates are adjusted to provide for complete reaction of the charge material, with 90 to 95 pct chlorine efficiency, and maintain a gas flow in the range of 0.4 to 0.6 ft per sec. The equipment consisted of a 3-in. diam mullite tube enclosed in an electric furnace. A bow-shaped 3/4 in. Saran tube fed the charge from an air lock type of feed hopper (to prevent the escape of the chlorine gas into feed bin) to the bottom of the bed. The charge rate was set by providing a small awiliary hopper below the feed hopper where a weighed portion of the charge could be discharged in a specified time interval into the main chlorine stream. The chlorine rate was measured by a flowmeter. The reaction tube was filled with a bed of Australian rutile ore, this restraining bed serving two purposes; i.e., it rapidly heated the fresh charge to the reaction temperature and retained the particles in the bed for a sufficient time for selective chlorination to proceed. Due to the fine particle size and open, porous structure of the charge, this reaction was almost instantaneous, and, with proper adjustment of feed and gas rates, very little fine material passed through the bed without reacting and only a very small fraction of the restraining bed was chlorinated. A typical reaction procedure was to fill the bench scale fluidized bed unit with a 1 kg charge of Australian rutile ore analyzing 95.5 pct TiO2, 0.6 pct FeO, a beach sand deposit 40 to 150 mesh size. When fluidized, the bed was approximately 2 ft in depth. The ore was fluidized with a 1:l mixture of chlorine and nitrogen at a rate of 0.40 ft per sec. This gas mixture was necessitated by the comparatively short bed depth; a larger unit, with a deeper bed, could be fluidized with chlorine alone without significant free chlorine loss. Feed rate was 8.0 g per min of beneficiated ilmenite analyzing 85.0 pct TiO2, 2.6 pct FeO plus 1.6 g per min of 20 to 60 mesh petroleum coke. The

Jan 1, 1962

By John D. Price

R. W. Campbell (Jones and Laughlin Steel Carp., Pittsburgh)—As usual John Price has presented an excellent paper. I know of no one who has devoted more time and conscientious thought to this subject than he has, and his efforts have produced scientific data and conclusions of real value. Results of similar studies made by the Jones and Laughlin Steel Corp. on the blending of Pennsylvania coals may be of interest. During 1935 the late F. W. Wagner and the present writer developed an empirical physical fuel value formula for evaluating the combined physical tests of metallurgical coke, see Table IV. In the development of the formula, the tumbler test, shatter test, screen test, and porosity of coke have been taken into consideration. Each of these tests brings out some physical property not expressed by the others, and in estimation of the importance of these tests as a medium for evaluating coke for the blast furnace, their worth has been graded as follows: It was thought that some additional penalty should be applied to cokes that do not show a uniform screen size, assuming that coke larger than 4 in. was not desirable and that this size was an indication of irregular size. Therefore the screen test factor is further corrected by applying a penalty of 1 pct for each 1 pct material greater than 4-in. size as shown by the screen test. The physical fitness of coke for blast furnace use depends upon four fundamental characteristics: l—gen-era1 strength, as indicated by the shatter test; 2— abradability, or the resistance of cell walls to reduction in size by attrition, as indicated by the tumbler test; 3—porosity; and 4—size and uniformity. Each of these characteristics is not of equal importance, but surely, in an attempt to determine an accurate physical value, the individual value of each should be taken into consideration. The formula is used as a yardstick, so to speak, in determining variations in the normal production of metallurgical coke and in making comparisons between normal coke and experimental blends with other coals. Table IV gives results of coking tests on raw and washed high volatile coals and these same coals with blends of coke breeze, anthracite coal, char and low volatile coals, all from Pennsylvania. The table also gives the source of the coals and coke breeze, as well as their proximate analyses. It will be noted that the washing of the raw high volatile coal increased the physical fuel value from 26.17 to 39.16, showing the effect of removing shale and slate which produces a detrimental fracturing and weakening of the coke. It is a well known fact that many Pennsylvania high volatile coals contain an excess of resinous material or binder which has a tendency to weaken the coke, owing to its high evolution of gases during carbonization. Tests were therefore made with coke breeze, an inert material, in an attempt to alleviate this condition. Blends of washed coal with 5 pct and 7.5 pct coke breeze collected from the coke plant quenching sump (82.9 pct through 1/8-in. screen) resulted in cokes with a physical fuel value of 20.75 and 16.73 respectively, lower than results obtained from 100 pct raw high volatile coal. It will be noted that the percentage of + 4-in. coke increased but that the tumbler test was very low. Undoubtedly better results could have been obtained if the coke breeze could have been crushed extremely fine. During World War II the government asked the coking industry to consider the use of anthracite coal as a substitute for high quality low volatile coal, which was extremely scarce at the time. The next series of tests was made with blends of raw and washed high volatile coals and 5, 10, and 15 pct Pennsylvania No. 5 buckwheat anthracite (100 pct through l/8-in. screen). It was necessary to use some raw high volatile coal in these blends because of insufficient washer capacity at the time. It will be noted that the physical fuel values

Jan 1, 1954

By Gordon E. Agar, David M. Hopstock

This paper describes the procedures and results of a series of experiments conducted to determine the depressing effect of sodium, calcium and magnesium ions on the amine flotation of quartz. It also presents an analysis of the experimental results by the electrical double layer theory. The flotation of quartz with primary amines has been practiced on a large scale in the phosphate industry for many years. Some glass sand —and recently iron ore — has also been treated by this flotation technique. These applications have been highly successful and demonstrate that a complete mastery of all the details of an operation is not needed to achieve an economic success. There are times, though, when it becomes important to recognize, both qualitatively and quantitatively, the effects of some previously ignored variables. The effects of cations on the amine flotation process, particularly those ions that contribute to water hardness and abound in sea water, are a case in point. In conjunction with the development of a cationic flotation reagent for separating quartz from apatite, it became necessary to quantify the influence of calcium and magnesium on the separation. In order to strengthen and broaden current understanding of the flotation process, the results were interpreted by means of the electrical double layer theory. THEORETICAL BACKGROUND Assume that, given the same equipment, procedure, and time, the recovery of quartz by amine flotation is a function of only the adsorption density of aminium ions in the Stern layer, i.e., that for any given adsorption density there exists only one recovery percentage. By the Stern-Grahame treatment of the electrical double layer,'-' for any ionic species in a solution in equilibrium with quartz,

Jan 1, 1969

CONTENTS PAGE PEIRCE, CARL-Making Rimmed Steel. Discussed by L. F. Reinartz. H. D. Hibbard, C. L. Kinney, Jr., A. H. Woodward, V. B. Buck, A. L. Feild, J. V. W. Reynders 1 SCHROEDER, F. W., and LARSEN, B. M.-Progress Report of the Effect of the Open-hearth Process on Refractories. Discussed by D. A. Lyon 12 KEATS, J. L., and HERTY, C. H.-Elimination of Metalloids in the Basic Open-hearth Process. Discussed by J. V. W. Reynders 14 Making Rimmed Steel Discussion of paper by CARL PEIRCE, presented at the New York fleeting and issued, as Paper No. 1563-C, with MINING AND METALLURGY, March, 1926. L. F. REINARTZ, Middletown, Ohio.-Mr. Carl Peirce has presented a valuable paper on a subject that has been very widely discussed in recent years, especially since the demand for high finish, deep drawing and other grades of sheet steel in the lower carbon ranges has become an important factor in the steel business. Steel of this analysis has been produced for many years, but the product for which it was made did not require the extra care in the steel plant that it does today. It must now be worked down into thin sheets for special purposes and undergo many severe finishing processes both in the steel mill and in the fabricating plants. Mr. Peirce's paper has outlined in a concise and logical manner the steps which must be taken in manufacturing such steels. The secret of successs is attention to details of well known steel practices. I agree with him that quality steels of this class cannot normally be made out of inferior raw materials. Scrap should be clean and if possible not too variable in analysis. Galvanized scrap or babbit are particularly objectionable. Scrap should be in such physical condition that undue delays are not encountered in charging the furnace. Limestone should preferably contain over 95 per cent. available calcium carbonate, and be free from clay or other foreign substances. Almost universal practice shows that 10 per cent. limestone is required for proper slag volumes to protect the metal from over oxidation. The use of 8 per cent. limestone makes the operation less fool-proof.

Jan 4, 1926

By M. R. Geer, H. F. Yancey

Four coals were treated in the Humphreys spiral concentrator, and the products were examined by float-and-sink and screen-sizing tests to determine fundamental performance characteristics. The efficiency of the separation between coal and impurity was shown to be influenced greatly by particle size.

Jan 1, 1950

THE morning session on mining methods with R. M. Raymond as chairman was devoted mainly to papers on explosives and the discussion of these papers. A paper on the numerical index of the re-sistance which rocks offer to the penetration of a drill bit was also read. The first paper, "Relation Between the Oxygen Bal-ance and Propulsive Strength of Eight Gelatin Dynamites" by G. St. J. Perrott, N. A. Tolch and J. E. Crawshaw, was presented by Mr. Perrott, super-intendent of the Pittsburgh Experiment Station of the U. S. Bureau of Mines. In this paper which is the beginning of a series of publications on explosives, Mr. Perrott stated that the attempt was made to put down in quantitative form the facts which have been known to explosive engineers for a long time. Eight samples of 40 per cent gelatin dynamite, with oxygen content varying from + 15 to - 36 per cent of the theoretical amount necessary to form complete combustion with all of the combustible elements were tested. The experimental work showed that a bal-anced explosive did not give the greatest propulsive strength-but the most favorable range was from - 8 to - 25 per cent oxygen. The experimental work also brought out the fact that the wrapper of a stick of dynamite enters quite completely into the explosive reaction, and gelatin dynamites from which the wrapper had been removed developed less strength than the a same explosive with the wrapper. The second paper, "Effect of Oxygen Balance of Gelatin Dynamites on the Gaseous Products of Det-onation," by G. W. James and G. St. J. Perrott, was also presented :by Mr. Perrott. The first portion of this paper is given over to a discussion of the relative merits of different types of apparatus for testing and analyzing the combustion products of dynamites. Three types were used (1) the Bichel gage, (2) the Crawshaw-Jones apparatus and (3) the Hercules tank. All three of these types were used in testing dynamites whose oxygen balance varied from-35 to + 6 per cent.

Jan 3, 1928