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By John Wellington Finch

INVESTIGATIONS by the Bureau of Mines of deposits containing strategic minerals were authorized by what has become known as the Strategic Materials Act (Public No. 117, 76th Congress, Chapter 190. 1st Session). A later act providing an appropriation for the first of four years through which the investigations are to be conducted was signed on Aug. 9, 1939. No time has since been lost as seven field projects already are being vigorously prosecuted, and two others no doubt soon will be in course of execution. Project engineers were at their stations within two days after funds had been made available. Crews have been hired; equipment and supplies have been purchased; 5 bids for diamond drilling have been obtained and the drilling has started base camps have been established: ground has been cleared; and several thousand feet of trenching, test-pitting, and sampling have already been done. At the Reno Experiment Station of the Bureau, a special metallurgical laboratory has been provided to make assays, analyses, and tests upon samples of ores from all projects under investigation.

Jan 1, 1939

By B. D. Harden

FOR over fifty years the Spanish mine, 21 miles northeast of Nevada City, in Nevada County, California, has been one of the Bradley properties. Between 1883 and 1889 it was operated by the late Frederick W. Bradley and P. R. Bradley. The ore averaged only about $1 a ton at that time but the mine was credited with a production of about $900,000 in that period. The property was then closed down until 1922, when the Bradley interests reopened it and continued development for the next nine years, when a 50-ton mill was built. This began operation in April, 1931. This was a selective flotation plant, with the tailing treated on Wilfley tables, and operated on ore from the No. 4 and No. 16 tunnel stopes. This ran from $3 to $6 in gold, 2 to 3 oz. of silver, copper 0.6 per cent, lead 1.5,

Jan 1, 1935

By Allen V. Heyl

This old district is a major zinc and lead source and minor copper and barite source. Ores are chiefly in the Galena Dolomite and in limestones and dolomites of the Decorah and Platteville Formations, all of Middle Ordovician age. Locally, deposits have been mined from Lower Ordovician dolomites and Upper Cambrian sandstones. Small deposits of lead, zinc, and iron sulfides have been found in Upper Ordovician Maquoketa Shale and in Lower and Middle Silurian Edgewood, Kankakee, and Hopkinton Formations. No post-Precambrian igneous rocks are known in the region, and the granitic and metasedimentary Precambrian basement rocks unconformably underlie the district at depths of 1500 to 2000 feet. The strata are gently flexed and faulted, probably largely the result of gentle compressive and rotational adjustments in the underlying crystalline basement, especially along lineaments between basement blocks. Folds of three orders ·of magnitude are recognized, and many related reverse, strike-slip, and normal faults of small to moderate displacements are present. Zinc-lead deposits are commonly linear, arcuate, or elliptical in plan. Most ore occurs as vein fillings in fractures and as breccia fillings and lining vugs, but some is in bedded replacements and impregnations of wall rocks. The ore is in shears, small reverse and bedding- plant faults, joints, and solution-slump structures related to intermediate and small folds. The main primary minerals in their general sequence of deposition are quartz, illite, dolomite, pyrite, marcasite, cobaltite(?), sphalerite, galena, chalcopyrite, millerite, barite, and calcite. Wall-rock alterations include solution of the carbonate rocks, silicification, dolomitization, clay alteration, and sanded dolomite. Oxygenisotope, trace-element, lead-isotope, and sphalerite- stratigraphy studies are in progress. Fluid inclusions in sulfide and gangue minerals are filled with concentrated brines at 120° to 40°C. Sulfides are directly replaced by supergene minerals above the water table at 50 to 100 feet in depth. In this relatively cool climate and limestone environment, smithsonite is in pseudomorphs after sphalerite; solution transport and redeposition of supergene minerals are rare. Ore genesis is postulated by rising hot-water solutions-a mixture of heated connate, magmatic, and meteoric waters.

Jan 1, 1968

By G. K. Manning, P. C. Rosenthal

USE of copper as an intentionally added alloy in steel and cast iron has rapidly expanded with-in the last fifteen years. It is estimated that in 1931 not more than 2000 tons of copper were so used; by 1941, however, this figure had grown to 13,000 tons. Tonnage figures during the war years have been restricted just as copper itself has been restricted, but copper-bearing cast irons and steels have played a part in the production of ordnance equipment. They are used in gun carriages, airplane landing-gear assemblies, scout cars, bulldozing equipment, army trucks, armor plate and many other instruments of war. These wartime applications have their counterpart in many peacetime applications; derricks, dredges, mine equipment, railway equipment, trucks, farm implements, automobiles, and tractors, all usually contain some parts made of copper-bearing steel or iron. An example of this is the Ford tractor which in 1940 contained over 300 lb. of copper-bearing steel castings. To this list should be added corrugated building sheet for exterior use most of which, at the present time, contains upward of 0.15 per cent copper. With the return to peacetime economy and the removal of wartime restrictions, it appears certain that copper cast irons and steels will find increasing application in civilian goods.

Jan 1, 1945

By AIME AIME

I am happy to welcome you to the twenty-third conference of the National Open-Hearth Committee, and our joint conference with the Blast Furnace Committee, of the American Institute of Mining and Metallurgical Engineers. It is appropriate that, for our fifteenth year anniversary, we should meet in the hotel and the city where this Open-Hearth Committee was inaugurated in 1925. At that first meeting, only a handful of men from a number of steel companies met to discuss ways and means to start a movement to improve the practical and metallurgical technique of open-hearth operations among independent manufacturers, as the United States Steel Corporation had carried on for many years.

Jan 1, 1940

By John T. Cumberlidge, Frederic M. Chace

Nickel-bearing saprolite developed during the early Tertiary over a northeast trending ultramafic body of Jurassic age near Riddle in southwestern Oregon. The principal nickel mineral is garnierite, but other complex nickel minerals may be present. There are two main ore bodies, an upper (older) one associated with the Klamath peneplain, and a lower (younger) one on the Sherwood peneplain. Saprolite constitutes the bulk of the ore and was probably derived from peridotite and dunite through chemical decomposition by downward percolating meteoric groundwater. Decomposition took place by net loss of MgO, SiO2, and Fe without a change in volume. Faults and joints provided permeable zones which localized saprolite development, and faulting may have helped preserve some ore from loss by erosion. Garnierite-chalcedony boxwork ore was deposited by meteoric groundwater along faults, joints, and at the level of former water tables. Boxwork ore is entirely supergene, the chemical constituents having been derived from higher in the soil profile. The saprolites show evidence of both supergene and residual enrichment in nickel. Red and yellow soil occurs as a capping over saprolite and boxwork, and was derived from them by chemical and mechanical decomposition. The present deposits are probably truncated remnants of a formerly thicker and much more extensive deposit which probably included laterite at the surface. The deposits started to form in the early Tertiary due to deep chemical weathering under sub-tropical to warmtemperature conditions. Early Tertiary ero~ion surfaces of low relief probably contributed to the predominance of chemical weathering over mechanical erosion. Alteration under present climatic conditions favors the formation of soil from saprolite rather than the formation of new saprolite from peridotite.

Jan 1, 1968

Jan 1, 1968

By AIME AIME

THE Annual Meeting-numerically the 162d meeting-of the American Institute of Mining and Metallurgical Engineers will be held at the Pennsylvania Hotel, 7th Ave. and 33d St., New York, Feb. 18-22, with the exception of the following events: the Mineral Industry Education Division will meet Sunday afternoon and evening at the Columbia University Men's Faculty Club, 400 West 117th St.; and a meeting of the Section Delegates, the annual business meeting of the Institute, and an executive session of the Board of Directors will be held in that order Tuesday afternoon in the Engineering Societies Building, 29 West 39th St., where the Directors will meet in the evening following their annual dinner to the Section Delegates. The Pennsylvania--one of the Statler group of hotels-was selected as headquarters because it has the physical equipment and facilities-for registration, technical sessions of all sizes, luncheons, social events, etc.-as well as the prominence and location desirable for an Institute annual meeting. (A tip for Tuesday afternoon and evening: You can walk underground from the Pennsylvania to within half a block of the Engineering Societies Building,)

Jan 1, 1945

By John T. Crawford

Introduction Loading and hauling systems are evaluated in open pit mining for new properties, expanding existing operations, changing systems or equipment, and equipment replacement analysis. The objective of such evaluations is to determine the equipment needed to handle planned tonnages at the lowest cash flow cost. Cash flow costs are used to combine capital outlays with operating and maintenance costs. Leasing costs could be substituted for capital costs with appropriate modifications to calculation procedures. These modifications will not be covered. This chapter will describe methods of evaluating loading and hauling systems, concentrating on some of the more often raised questions concerning quantitative data. While the methods described are not the only ones in current use, they have a record of proven reliability. The shovel and haulage truck system is used In the examples because of its common use in open pit mines. In medium to large open pit mines, electric shovels and diesel-electric drive haulage trucks are normally used. The basic ideas presented in this chapter apply to all loading and hauling systems, with appropriate modifications. The process of performing a shovel and haulage truck evaluation can be time-consuming and tedious because of the quantity of data involved, but it is not particularly difficult. The examples used to Illustrate shovel and haulage truck evaluation are based on a hypothetical open pit mine operating 350 days per year producing 31 750- 000 t (35,000,000 st, 100,000 stpd) annually, of which 11 110 000 t ( 12,250,000 st, 35,000 stpd) are ore. Selection of the optimum shovel and haulage truck fleets will be shown. The principal sources of data for the examples or any other equipment evaluation are equipment manufacturers and actual operations. Whenever possible, actual operating experience should be used to verify estimates. The quantitative data presented herein are unrelated to a specific existing mining operation.

Jan 1, 1979

By H. H. Power

THE PETROLEUM DIVISION of the A.I.M.E. continued with its diversified activities during 1.935. Sessions at the New York meeting in February were devoted to production engineering, domestic and foreign oil production, and petroleum economics. The symposiums on domestic and foreign production proved their increased usefulness. The data accumulated for 1935 were added to those published during prior years in "Petroleum Development and Technology." A joint session on the use of metals in the petroleum industry was held by the Institute of Metals, Iron and Steel, and Petroleum Divisions. W. S. Farish, chairman of the board of the Standard Oil Co. (N. J.), was the principal speaker at the annual dinner. The October meeting, held in Hous¬ton, was characterized by an excellent program and large attendance. Four sessions were devoted to problems in estimating reserves, reservoir energy, properties of drilling muds, electrical logging, water flooding, and other subsurface studies. Foreign representatives of the Anglo-Persian Oil Co. presented a paper on surface tension and specific gravity of crude oil under reservoir conditions. The address by President Buehler, the dinner at San Jacinto Inn, a trip to various lo

Jan 1, 1936

By T. W. Beck

Roof bolter occupations in underground coal mines continue to experience overexposure to respirable dust. One potential source of dust in roof bolting operations is the exhaust from the roof bolter dust collection system. A wet exhaust conditioner (water box) has been developed to reduce dust emissions from the exhaust of the vacuum dust collection system on roof bolting machines. The exhaust conditioner consists of a muffler chamber and a water chamber with four internal partitions to direct airflow over the surface of the water. The National Institute for Occupational Safety and Health conducted a series of laboratory tests to assess the respirable dust capture ability of this device as compared to the standard exhaust muffler. To determine the dust collection efficiency, both devices were placed in the exhaust stream of a simulated roof bolter dust collection system. Gravimetric samplers were operated upstream and downstream of the exhaust conditioner and muffler to evaluate the ability to capture both respirable coal and limestone dust. Researchers observed a 41 % reduction in dust concentrations for the water exhaust conditioner in the laboratory configuration. Significant levels of dust deposition in the sampling chambers may have contributed to this effective capture rate.

Jan 1, 2012

By B. B. Gottsberger

IT SEEMS strange that so many years after the pas¬sage of the first acts requiring registration or licensing of engineers, so few members of the mining branch of the profession are aware of what has taken place. Laws regulating the practice of engineering have now been passed in 19 states of this country, and in many others, such legislation has been proposed. That such laws are necessary for the protection of life, health and property, as is stated in most of them, is doubted by many. That the standing of the engineering profession will be improved by them is certainlyy open to question. That such laws are a welcome addition to the regulation of business by governmental agency, is not likely to be a general opinion. That once more, and in spite of appeals to engineers to interest themselves in affairs of government, an active minority has succeeded in imposing its will on a passive majority, seems but too true. However, the laws are there and information regarding them should be of use and interest to those most directly concerned.

Jan 1, 1921

By F. N. Rhines, A. S. Nemy

The mode of high-temperature tertiary creep of 523-0 aluminum alloy was found to be strongly stress dependent. The occurrence of necking and/or fissures during tertiary creep exhibited a sequence with varying stress, wherein fissures with no necking occur at a minimum stress and necking with no fissures occur at a maximum stress. At an intermediate stress, tertiary creep begins without necking but with fissures in a region just beneath the external surface, followed by necking and the development of fissures along the axis of the specimen. The results are interpreted in terms of grain boundary gliding and the hydrostatic stresses produced by restraints to grain boundary gliding. THERE appear to be two possible reasons for the existence of a period of accelerating elongation prior to rupture during high-temperature creep in metals; namely, 1) a change in the structure of the metal itself, leading to a change in its response to loading, and 2) a reduction in the cross section of the metal resulting in a higher unit loading. Howe,' by annealing and retesting broken low-temperature creep specimens, found that irreparable damage is done once a metal is subjected to creep. Andrade2 first pointed out the association between the reduction in cross section and the increase in creep rate. The present research was designed to investigate both of these factors by retesting specimens machined from material which had been subjected to high-temperature creep testing short of rupture. EXPERIMENTAL METHOD An aluminum alloy, 52s-0, was selected for these studies because it is constitutionally simple, is strong enough to be relatively insensitive to mechanical damage during machining,3 and undergoes accelerating creep in a convenient temperature range. This alloy is hardened by 2.6 wt pct Mg in solid solution and is not subject to overaging effects; it has a very small quantity of an insoluble impurity phase, Mg2Si, finely dispersed throughout its micro-structure. Creep specimens, similar in design to ASTM 0.252-in. tensile specimens, were machined from 3/4-in. round stock and the surfaces were electro-polished. A 24-hr anneal at 500°C was then applied to stabilize the grain size to an average diameier of 0.27 mm. Subsequent heating for as long as 700 hr at the intended test temperatures produced no change in the tensile properties, indicating a well-stabilized state of the material. Corresponding to each of the typical testing conditions listed in Table I, one creep specimen was tested to destruction and this test was employed as a guide in the selection of times for subsequent tests. Duplicate creep tests were then run to various points along the creep curve to produce specimens which were used to determine changes in mechanical properties and microstructures. The latter were examined at the midsections of the specimens. Other specimens were tested to various stages of tertiary creep, after which they were remachined to new cylindrical test specimens, electropolished and re-tested in creep. RESULTS The major findings of this investigation may be illustrated by a comparison of the results of three sets of creep tests. These were run at 400°C at three stress levels, namely 750, 1000, and 1500 psi. In presenting these results in Figs. 1, 5, and 8, the creep curves are given in pairs: That curve of each pair which is drawn through filled circles corresponds to the initial test, and the curve drawn through open circles (and designated by - R) represents the result of retesting the same specimen after machining to a new cylindrical surface. The load was readjusted to the original unit stress at the beginning of each retest.

Jan 1, 1960

By Finney, W. R.

MUCH has been said and written of the "Big Inch," of the terrific obstacles encountered in its construction, of the colorful and tough men engaged in its building, but little has been publicized of the engineering and economic problems behind the scenes. Long before Pearl Harbor it was apparent to the petroleum industry that a critical oil shortage could be expected along the Atlantic seaboard, owing to delay in tanker deliveries as a result of convoy movements, and to allocation of vessels for foreign shipments. This area, with a normal consumption of approximately 1,800,000 barrels per day of oil and products, was almost entirely supplied by tanker. Pipe lines supplied an average of only 20,000 barrels per day in 1939, 40,300 barrels per day in 1940, and 55,000 barrels per day in 1941. A small amount of oil and products was also delivered via barge.

Jan 1, 1943

By Willard P. Ward

SOME TIME in the year 1874 or 1875, I conceived the idea that spiegeleisen might be made -in a blast furnace from ores that were not carbonates, and which did not contain both manganese and iron in the same ore. Up to this time, such ores had formed the basis of all the spiegel that had been produced; and all the ferromanganese that was on the market before 1875 was made in crucibles, and cost about 00 per ton, for 80 per cent. Mn. I consulted the great steel metallurgist of the day, Alexander Holley, who listened attentively to what I had to say, and told me he did not think my plan was practical, so I abandoned it for the time being. But I was so stubborn that I could not get the notion out of my head. It seemed to me that a good metallurgist should be able to work the thing out in some way. I had already had some experience in smelting refractory lead ores in Utah, and was young and not lacking in self confidence, so after waiting a bit, I got Anton Eilers, the best all-around metallurgist I knew, and J. H. Bramwell, the best iron blast-furnace man I knew, both intimate friends of -mine, to come to my place in Bartow County, Georgia, and look over things. They remained for several days, and made all the examination they thought necessary; and they also advised me to give up the project, and either to keep the furnace running on car-wheel iron or to blow it out. After my talk with Holley, I improved my plant in several ways. I closed the top of the furnace, put in a hot-blast stove, a steam boiler and a Weimer blowing-engine which gave me blast enough, at a pressure high enough for all the requirements of, the furnace, and which I could bring up to a temperature of 600° to 700° F.

Jan 1, 1921

Jan 1, 1959

By Lewis Carroll

AS he contemplates the numerous good things the hard-working committees have evolved for the 140th Meeting of the Institute, the Editor knows just how the walrus felt when he uttered his memorable, if somewhat lugubrious lines. For there are the Annual Reception and Dinner at the Commodore, 'the Gold Supply Symposium, the luncheons, general and special, and the Annual Institute of Metals Lecture, a Round Table on Iron Ore and a wonderful Informal Dance at the Grand Central Art, Gallery, substantial general sessions, a Smoker-and many other things. -Old, friends and new, reminiscences and confidential chats, horizons pushed back by new information and adjusted perspectives, courage revived and ambitions stimulated-one with a flair for the modernistic might make something-or nothing-of the kaleidoscopic preview 'of the coming Annual Meeting.

Jan 1, 1931

By D. J. Mack, R. E. Reiswig

Six examples of the peritectoid transformation were selected from the literature and studied by the method of isothermal transformation. The kinetics and mechanisms of five of the examples are presented as TTT diagrams and photomicrographs. The exist-enc- of a peritectoid in the sixth case is doubtful. ALTHOUGH the peritectoid transformation per se has been known for many years, no precise published data exist concerning the kinetics or mechanisms involved in transformations of this type, except for the brief treatment by Rhines, et al. 1,10 Bearing in mind the fact that investigations of recent years are uncovering more and more peritectoids and suspected peritectoids, a thorough study of the well-established peritectoids appeared to be in order. It was for this reason that a study of the kinetics and morphological mechanisms of six binary peritectoids was undertaken. The six peritectoids selected from the literature for study were those reported at 7.02 wt pct Al-Ag, 26.0 wt pct Sb-Cu, 30.5 wt pct Sb-Cu, 32.3 wt pct Sn-Cu, 8.35 wt pct Si-Cu, and 21.2 wt pct Al-Cu. These selections were based on availability and purity of components, ease of preparation and heat-treatment, and estimated reliability of the available equilibrium diagrams in the regions of interest. EXPERIMENTAL PROCEDURE The alloys used in this investigation were induction melted in electrode-grade graphite and chill-cast in cast-iron split molds. In all cases, the alloys were so brittle that they could easily be broken into samples weighing 1 or 2 g. Chemical analyses showed that the alloys used were close to the respective peritectoid compositions reported in the literature and that the impurity levels were low in all cases. Metallographic examination showed uniform distributions of phases in all samples, indicating uniformity of composition in the samples studied. Isothermal transformation studies were carried out in fused-salt media, using the familiar inter-rupted-quench method. Uniformity of temperature in the salt baths was maintained by continuous stirring with a stainless-steel agitator. On the basis of actual observations of the temperature fluctuations, the estimated temperature control was + 10C for the Ag-Al and Cu-Sb alloys and ±30C for the Cu-Sn, Cu-Si, and Cu-Al alloys. The accuracy of all temperature measurements was estimated to be ±1°C. It was found necessary to mount metallographic specimens of the Ag-Al alloy in cold-curing methyl methacrylate, since the temperatures encountered in mounting in bakelite or lucite caused an appreciable degree of transformation to the ß phase. For the other alloys, wood-flour-filled bakelite mounts were used to avoid extraneous X-ray diffraction lines during the later examination of the metallographic specimens on a Norelco Geiger-counter d if f r ac tomete r. In the X-ray diffraction procedure, agreement between the published diffraction patterns and those obtained in this study was good. This was particularly important for phase identification, since the literature contained little in the way of micrograph description in some cases. Etching of the silver-aluminum alloy for metallographic examination was done by swabbing with either of the following reagents: 1) 10 g CrO3, 1 g (NH4), SO2, 0.5 g NH4NO3, 100 ml H2O, or 2) 10 ml NH4OH, 1 ml 20 pct KOH, 4 ml 3 pct H2O2, 5 ml H2O. The other alloys were etched with the usual bichromate etchant: 2 g K2Cr2O7, 1.5 g NaC1, 8 ml conc. H2SO4, 100 ml H20 (swabbed vigorously). EXPERIMENTAL RESULTS A) The Ag-Al peritectoid at 7.02 wt pct Al— The phase equilibrium involved in this peritectoid is shown in Fig. I.2 The phase boundaries in the vicinity of the peritectoid were most comprehensively established by Hume-Rothery, et al,3 who placed the equilibrium temperature at 448 °C and the equilibrium compositions of the a ß' and y phases at 6.11, 7.02, and 7.24 wt pct Al, respective The alloy used in this study analyzed4 6.95 wt pct A making it slightly hypoperitectoid according to the accepted equilibrium diagram. The rate of the transformation a+ y — ß' varies rapidly with degree of undercooling below the equilibrium temperature, passing through a maximum in the vicinity of 350°C. Thus the TTT dia-

Jan 1, 1960

By O. F. Kammerer, W. E. Miller, D. H. Gurinsky, J. Sadofsky, J. R. Weeks

Zirconium and titanium inhibit solution mass transfer of steels by liquid bismuth, mercury, and lead. It is shown that in bismuth and mercury, these adsorb on the surface of the steels and subsequently react with nitrogen and possibly carbon from the steels to form inert, adherent surface layers of ZrN, TiN, or TiN + Tic. Data are presented which describe the condition under which thase deposits form. These inhibitors decrease the solution rate of iron into bismuth, and require a higher supersaturation for precipitation of iron from bismuth. USE of the low-melting heavy metals (bismuth, lead, mercury, and their alloys) as coolants has been limited because solution mass transfer of steels occurs in these liquids; i. e., iron dissolves in the hot sections of the heat transfer circuit and deposits in the colder sections. The rate of solution of iron and the temperature coefficient of solubility are sufficiently great to cause complete or partial stoppage by the deposition in the coldest section of a closed circuit in finite time, even though the actual solubilities are extremely low. In the development of the mercury vapor turbine by the General Electric Co., Nerad and his associates1 discovered that the addition of as little as 1 ppm Ti or Zr to magnesium-deoxidized mercury reduced the mass transfer of ferrous alloys by mercury to a negligible amount. Reid2 reported that titanium was detected chemically on the surface of steels contacted with this mercury alloy in amounts varying from 2.0 to 2.6 mg per sq in., the greatest amount being found in the hottest portion of the circuit. Reid stated that the titanium forms the intermetallic compound Fe2Ti by reaction with iron on the surface of the steels. This compound was presumed to be highly insoluble in mercury. More recently, El-gert and Egan3 have reported a greater than 100-fold reduction in the rate of mass transfer of a 5 pet Cr steel by liquid bismuth upon the addition of titanium (in excess of 50 ppm) and magnesium (350 ppm) in the liquid metal, during experiments performed in thermal convection loops* over the temperature differential 700° to 615° C. Also, Shep-ard and his associates' have reported that the addition of titanium to liquid bismuth and Pb-Bi eutec-tic produced a marked decrease in the rates of solution of both iron and chromium from type 410 steel capsules under static conditions. This inhibiting effect increased with repeated reuse of the capsules. Tests performed in this laboratory under carefully controlled conditions have shown that the addition of zirconium and magnesium, or titanium and magnesium, to liquid bismuth or lead greatly reduces the rate of mass transfer of chromium alloy steels and carbon steels in thermal convection loops with a maximum temperature of 550°C.5-9 The present paper will review the data obtained to date at this laboratory on the behavior of iron and steels in contact with liquid bismuth alloys containing titanium or zirconium, and will attempt to explain the role of the above additives in reducing solution mass transfer. Reaction between the Zirconium or Titanium Dissolved In Liquid Bismuth and an Iron or Steel Surface Reaction between Zirconium Dissolved in Bismuth and the Surface of Pure Iron-—A small pure iron crucible (analyzed by the supplier to contain 0.8 ppm N was contacted with bismuth containing approximately 0.1 pet Mg and varying amounts of a radioactive zirconium tracer. The crucible was then inverted at the temperature of contact. The thin residual layer of adherent bismuth was dissolved in cold, concentrated nitric acid. The crucible surface and the solidified bismuth were then analyzed for radioactive zirconium. An analysis of the activity loss on the crucible surface and the weight loss of the crucible during the nitric acid treatment showed that the acid treatment removed the zirconium that had originally been dissolved in the adherent bismuth, but not any zirconium that may have reacted with the crucible surface. The crucible was then pickled in warm aqua regia to remove all surface activity, hydrogen-fired at 600°C, and recontacted with a new liquid alloy. The results of the experiments contacted 1 hr at 450°C show, Fig. 1, a Langmuir-type adsorption with an adsorption free energy of approximately 17 keal per g atom Zr.5 This deposit was estimated to contain 1 atom of zirconium for each 7 to 8 iron atoms on the crucible surface, assuming a surface roughness factor of the pickled crucibles to be five. Increasing the temperature to 520°C caused consi-

Jan 1, 1959

By R. M. Hudson, P. E. Perry

Weight-gain data obtained by nitriding low-carbon sheet steel in an amrnonia CNH,) atmosphere indicated that the process obeyed a parabolic rate law. The calculated actization energy for nitriding in the range 964" to 1268°F agreed reasonably well with published data. At 1358"F, rate data indicated that the activation energy decreased. Weight-gain data obtained by uszng mixtures of NH3 -Nz at 1268°F containzng jrom 10 to 100 zol pct NH3 also obeyed a parabolic rate law. The rate of 'nitriding increased with an increase in the NH3 content of the gas Mixture. It is well-known that steel heated in gas mixtures containing ammonia (NH3) takes up much larger quantities of nitrogen than steel heated in nitrogen, both gases having a total pressure of 1 atm;' this phenomenon can presumably be attributed to the catalytic decomposition of NH3 on the steel surface to furnish nascent (monatomic) nitrogen. This process was studied bv Brunauer. Jefferson, Emmett, and Hend-ricks at furnace temperatures of 752" and 831°F2 using mixtures of NH3 in Hz. Englehardt and wagner3 reported that, at a furnace temperature of 914°F and under their experimental conditions, both nitriding and denitriding were controlled by the rate of gas-metal reactions at a steel surface rather than by the rate of diffusion of nitrogen in iron. The present study was undertaken to obtain information on the kinetics of nitriding low-carbon steel strip at higher temperatures so that practical rates for short-time strip-annealing treatments could be estimated. Variables studied included time: temperature, and NH, content in the annealing atmosphere. Mechanical and chemical characteristics of steel nitrided in this manner will not be considered in the present article. MATERIALS AND EXPERIMENTAL WORK The samples used were from a commercial low-carbon steel, 0.0244 cm thick, in the cold-reduced condition. The chemical composition of this steel is given in Table I. Panels were cut to 5.1 by 17.8 cm, degreased in toluene, and weighed just before treatment. Four specimens were nitrided under each of the experimental conditions. A study was made of the nitriding rate of steel in a 100 vol pct ammonia atmosphere, 740 mm pressure, at five specific temperatures within the range 964" to 1358°F. The nitriding rates of steel in ammonia-nitrogen gas mixtures containing 10, 18, 26, 50, and 100 vol pct ammonia, 740 mm total pressure, at 1268°F were also determined. All atmospheres used were dried by successively passing them through drying towers packed with soda lime and with Linde Molecular sieve Type 4A. Quoted gas compositions refer to those entering the furnace. Specimens were held in the constant-temperature zone of a vertical annealing tube furnace for times of 14, 3, 5, 10, or 15 min. Gas flow rates were maintained at 3.8 cu ft per hr, which was nineteen volume changes per hour for the system used. The rate of flow was selected to provide a high level of free NH3 for cracking on the steel surface where the ammonia gas is most effectively used as a nitriding agent. The vertical annealing tube furnace consisted of a Hevi-Duty tube furnace with a 2 1/2-in.-ID mullite ceramic high-temperature tube. The constant-temperature zone (controlled within 10°F) was about 10 in. long. After each specimen was degreased, a hole was punched in one end, for attaching the specimen by hook to a chain so that it could be lowered into or raised from the high-temperature portion of the tube by means of a power-driven winch. A stainless-steel access port with O-ring seals was connected by suitable glass-to-metal seals to the cool upper portion of the furnace tube. After the weighed specimen was placed in the access port, the furnace tube was evacuated to approximately 10"3 torr, and then the system was flushed thoroughly with the atmosphere under study. When the gas flow rate and constant-temperature zone of the furnace were established, the specimen was lowered into the constant-temperature zone. The atmosphere flowed from the top to the bottom of the vertical furnace tube and was then vented. For all these runs, during the first 3 min of the time the specimen was in the constant-temperature zone of the furnace the specimen was heating up to the tempera-

Jan 1, 1970